CN103333056B - Method and device for deeply removing sulfide in MTBE - Google Patents
Method and device for deeply removing sulfide in MTBE Download PDFInfo
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- CN103333056B CN103333056B CN201310300138.9A CN201310300138A CN103333056B CN 103333056 B CN103333056 B CN 103333056B CN 201310300138 A CN201310300138 A CN 201310300138A CN 103333056 B CN103333056 B CN 103333056B
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Abstract
The invention provides a method for deeply removing sulfide in MTBE (Methyl Tert Butyl Ether). The method comprises the following steps: the sulfur-containing MTBE enters into a tower kettle from the bottom of a sulfide absorption rectifying column; the sulfur-containing MTBE passes through a separation absorption section arranged at the lower part of the rectifying column and a depth absorption section arranged at upper part of the rectifying column from bottom up after heated; when the sulfur-containing MTBE passes through the separation absorption section, pneumatolytic MTBE mixture is in countercurrent contact with liquid phase sulfide absorbent led in separation absorption section of the rectifying column to accomplish absorption; when the sulfur-containing MTBE passes through the depth absorption section, the pneumatolytic MTBE mixture is dispersed to enter liquid phase absorbent, the absorption is completed through gas-liquid two-phase depth contact, the absorbent which absorbs sulfide and MTBE product after deep desulfurization are obtained finally. According to the method provided by the invention, the defects of MTBE product rectifying desulfurization technology that the range of sulfide content is wider and sulfide content with low boiling point is higher existed in a conventional technology are overcame, so that the deep desulfurization to MTBE product is realized. The invention further provides a sulfide absorption rectifying column used by the method.
Description
Technical field
The invention belongs to technical field of petrochemical industry, 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 liquefied petroleum gas (LPG) C-4-fraction, as gasoline dope, has excellent anti-knocking property.The compatibility of it and gasoline is good, and water suction is few, environmentally safe.As organic synthesis raw material, can the iso-butylene of preparing high-purity.
Sulphur in the MTBE product that MTBE device is produced is mostly organosulfur, mostly be mercaptan, thiophene, sulphur ether material, because raw liquefied petroleum gas is different, MTBE medium sulphide content has the diversity of composition, the feature of sulphur content a wider range, especially, under the situation that lower boiling sulfide content is higher in MTBE, by 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 prior art, the particularly deficiency of the MTBE product rectifying desulfurization technology that lower boiling sulfide content is higher, develop a kind of one-piece absorbent device of spiral-screen column and the method with double absorption function, thus realize 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, comprise the following steps: sulfur methyl tertiary butyl ether (MTBE) enters tower reactor from sulfide absorption distillation tower bottom, from bottom to top through being located at the separate absorbent section of rectifying tower bottom and being located at the degree of depth absorber portion of rectifier after heating; Through separate absorbent section, the MTBE mixture of gasification completes absorption with the liquid phase sulfide absorption agent counter current contact introducing rectifying tower separate absorbent section; Through degree of depth absorber portion, the MTBE mixture of gasification is dispersed to liquid absorbent inside, completes absorption by gas-liquid two-phase deep contact, the absorption agent of the sulfide that has finally been absorbed and the MTBE product through deep desulfuration.
In the preferred scheme of one of the present invention, comprise further and the absorption agent absorbing sulfide obtained in described sulfide reboiled absorber is discharged from the bottom of described separate absorbent section and degree of depth absorber portion respectively, enter absorbent regeneration tower, after regenerator column process, the sulfide that reclaiming tower top obtains, returns the absorbent regeneration obtained at the bottom of recovery tower to sulfide reboiled absorber simultaneously and recycles.
In the another kind of preferred scheme of the present invention, comprise further by obtain in described sulfide reboiled absorber through deep desulfuration MTBE product through cooling after, part MTBE backflow enters described sulfide reboiled absorber, another part MTBE is through MTBE product introduction products pot, and reflux ratio is: 0.2 ~ 10.
In another preferred scheme of the present invention, described sulfide reboiled absorber preferred structure integrated secondary reboiled absorber as shown in Figure 2, it is divided at the bottom of tower from bottom to top, separate absorbent section 201, degree of depth absorber portion 202 and tower top; Described separate absorbent section 201 bottom column wall is provided with the sulfur-bearing MTBE opening for feed 206 be connected with the dispersion pipe in tower reactor, and in the middle part of separate absorbent section 201, tower wall is provided with separate absorbent section absorption agent opening for feed 205; The distribution house steward 210 of top closure is provided with in described degree of depth absorber portion 202, this distribution house steward 210 lower ending opening is in separate absorbent section 201 top and to project up degree of depth absorber portion 202 inner, draws one or more arm communicate with the dispersion pipe bottom degree of depth absorber portion 202 from described distribution house steward 210; In the middle part of described degree of depth absorber portion 202, tower wall is provided with degree of depth absorber portion absorption agent opening for feed 204, and described degree of depth absorber portion 202 bottom column wall is provided with degree of depth absorber portion absorption agent discharge port 209; Communicate by means of only the arm of described distribution house steward 210 and extraction thereof between described separate absorbent section 201 and degree of depth absorber portion 202; Separate absorbent section absorption agent discharge port 207 is provided with at the bottom of described rectifying tower; Described rectifying tower tower top is provided with MTBE gas phase discharge port 203.
Further in preferred sulfide absorption distillation tower structure, be provided with phegma mouth 208 at described separate absorbent section 201 top drum wall.
Sulfide reboiled absorber column plate of the present invention is located in rectifying tower, and described stage number N is: 1 < N≤200, preferably 5≤N≤50.
Described dispersion pipe can adopt calandria or annular tube type.
The degree of depth absorber portion 202 on sulfide reboiled absorber top of the present invention and separate absorbent section 201 tower reactor of bottom can also load dumped packing further.
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 θ type filler.
The absorption agent used 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 wherein two or more mixture.
In the inventive method, absorption agent add-on and the MTBE inlet amount mass ratio of described separate absorbent section are preferably 0.5 ~ 3:1.
In the inventive method, sulfur methyl tertiary butyl ether (MTBE) can adopt the form of gas phase, liquid phase or gas-liquid mixed phase to disperse charging from tower reactor when separate absorbent section enters reboiled absorber.
When the present invention uses the rectifying tower of above-mentioned preferred structure as sulfide reboiled absorber, as shown in Figure 1, the methyl tertiary butyl ether of sulfur-bearing enters the separate absorbent section tower reactor of structure integrated secondary reboiled absorber 103 as shown in Figure 2 from MTBE opening for feed 102, feed pressure is 0.1 ~ 1.5MPa, feeding temperature is 40 ~ 150 DEG C, tower reactor control temperature 65 ~ 90 DEG C, METB mixture under thermogenic action with integrated secondary reboiled absorber 103 in the middle part of the liquid absorbent counter current contact that added by separate absorbent section absorption agent opening for feed 101, removing of most of sulfide is completed in separate absorbent section, the MTBE removing most of sulfide enters the degree of depth absorber portion on integrated secondary reboiled absorber 103 top by the distribution house steward 210 in Fig. 2 and with the arm of dispersion pipe UNICOM bottom degree of depth absorber portion again, it is inner that absorption agent is imported degree of depth absorber portion by the absorption agent opening for feed in the middle part of degree of depth absorber portion, and submergence is arranged on the dispersion pipe bottom degree of depth absorber portion, divide sulfide in the MTBE shed after absorption agent secondary deep absorbs by dispersion pipe in degree of depth absorber portion, qualified MTBE enters overhead condenser 104, tower top control temperature is 50 ~ 60 DEG C, pressure is normal pressure, after overhead condenser 104 cools, temperature is that the MTBE of 40 ~ 50 DEG C enters return tank 105, reflux pump 107 is entered through return tank outlet pipe 106, act on next section MTBE at reflux pump 107 and enter integrated secondary reboiled absorber 103 through return line 110, another part MTBE enters products pot through MTBE products export pipe 111, reflux ratio is 0.2 ~ 10, bottom sulfur absorbing agent automatic integral double absorption rectifying tower 103 tower reactor and tower top degree of depth absorber portion, absorbent regeneration tower 113 is entered through separate absorbent section absorption agent to be regenerated outlet pipe 108 and degree of depth absorber portion absorption agent outlet pipe 112 to be regenerated, during regenerator column 113 normal pressure: bottom temperature is 200 ~ 250 DEG C, tower top temperature is 90 ~ 160 DEG C, during decompression: bottom temperature is 60 ~ 90 DEG C, tower top temperature is 50 ~ 60 DEG C, and the sulfide of removed overhead, through regenerator column overhead condenser 114, is delivered to sulfur recovery system by sulfide outlet pipe 115, after regeneration at the bottom of tower, absorption agent is after absorbent regeneration condenser 117, and the absorption agent opening for feed 101 entered in the middle part of integrated secondary reboiled absorber 103 recycles.
The present invention also provides a kind of sulfide reboiled absorber for deep removal MTBE medium sulphide content, can by its called after " integrated secondary reboiled absorber ", as shown in Figure 2, its structure be divided at the bottom of tower from bottom to top, separate absorbent section 201, degree of depth absorber portion 202 and tower top; Described separate absorbent section 201 bottom column wall is provided with the sulfur-bearing MTBE opening for feed 206 be connected with the dispersion pipe in tower reactor, and in the middle part of separate absorbent section 201, tower wall is provided with separate absorbent section absorption agent opening for feed 205; The distribution house steward 210 of top closure is provided with in described degree of depth absorber portion 202, this distribution house steward 210 lower ending opening is in separate absorbent section 201 top and to project up degree of depth absorber portion 202 inner, draws one or more arm communicate with the dispersion pipe bottom degree of depth absorber portion 202 from described distribution house steward 210; In the middle part of described degree of depth absorber portion 202, tower wall is provided with degree of depth absorber portion absorption agent opening for feed 204, and described degree of depth absorber portion 202 bottom column wall is provided with degree of depth absorber portion absorption agent discharge port 209; Communicate by means of only the arm of described distribution house steward 210 and extraction thereof between described separate absorbent section 201 and degree of depth absorber portion 202; Separate absorbent section absorption agent discharge port 207 is provided with at the bottom of described rectifying tower; Described rectifying tower tower top is provided with MTBE gas phase discharge port 203.
Further in preferred sulfide absorption distillation tower structure, be provided with phegma mouth 208 at described separate absorbent section 201 top drum wall.
Sulfide reboiled absorber column plate of the present invention is located in rectifying tower, and described stage number N is: 1 < N≤200, preferably 5≤N≤50.
Described dispersion pipe can adopt calandria or annular tube type.
The degree of depth absorber portion 202 on sulfide reboiled absorber top of the present invention and separate absorbent section 201 tower reactor of bottom can also load dumped packing further.
The two-part secondary deep sulfur method that the present invention absorbs by adopting separate absorbent and the degree of depth, the MTBE desulfurization degree of acquisition is significantly improved, and in addition, the inventive method also has the following advantages compared with the prior art:
(1) 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 in the situation that MTBE medium sulphide content content is wider, sulfide content 600 ~ 1000 μ g/g.
(4) MTBE yield and desulfurization degree high, final sulphur content 10 below μ g/g, MTBE object product yield is greater than 99.8%.
(5) MTBE desulfurization process is simple, invests low.
Accompanying drawing explanation
The process flow sheet of the methyl tertiary butyl ether of Fig. 1 described by embodiment 2-5 (MTBE) integrated secondary reboiled absorber deep desulfuration.
In Fig. 1, description of reference numerals is as follows: 101, separate absorbent section absorption agent opening for feed; 102, MTBE opening for feed; 103, integrated secondary reboiled absorber; 104, reboiled absorber overhead condenser; 105, reboiled absorber return tank; 106, return tank outlet pipe; 107, reboiled absorber reflux pump; 108, tower reactor absorption agent outlet pipe to be regenerated; 109, reboiled absorber tower bottom reboiler; 110, return line; 111, MTBE products export pipe; 112, degree of depth absorber portion absorption agent outlet pipe to be regenerated; 113, absorbent regeneration tower; 114, regenerator column overhead condenser; 115, sulfide outlet pipe; 116, well heater at the bottom of regenerator column tower; 117, absorbent regeneration condenser.
Fig. 2 is the integrated secondary reboiled absorber structural representation of the embodiment of the present invention 1.
In Fig. 2, description of reference numerals is as follows: 201, separate absorbent section; 202, degree of depth absorber portion; 203, MTBE gas phase discharge port; 204, degree of depth absorber portion cyclic absorption agent opening for feed; 205, separate absorbent section cyclic absorption agent opening for feed; 206, sulfur-bearing MTBE opening for feed; 207, separate absorbent section cyclic absorption agent discharge port; 208, phegma mouth; 209, degree of depth absorber portion cyclic absorption agent discharge port; 210, degree of depth absorber portion MTBE distribution house steward.
Embodiment
Embodiment 1
For a rectifying tower for deep removal MTBE institute sulfur compound, be integrated secondary reboiled absorber as shown in Figure 2, its structure is divided at the bottom of tower from bottom to top, separate absorbent section 201, degree of depth absorber portion 202 and tower top; Described separate absorbent section 201 bottom column wall is provided with the sulfur-bearing MTBE opening for feed 206 be connected with the calandria dispersion pipe in tower reactor, in the middle part of separate absorbent section 201, tower wall is provided with separate absorbent section absorption agent opening for feed 205, and separate absorbent section 201 top drum wall is provided with phegma mouth 208; The distribution house steward 210 of top closure is provided with in described degree of depth absorber portion 202, this distribution house steward 210 lower ending opening is in separate absorbent section 201 top and to project up degree of depth absorber portion 202 inner, draws one or more arm communicate with the calandria dispersion pipe bottom degree of depth absorber portion 202 from described distribution house steward 210; In the middle part of described degree of depth absorber portion 202, tower wall is provided with degree of depth absorber portion absorption agent opening for feed 204, and described degree of depth absorber portion 202 bottom column wall is provided with degree of depth absorber portion absorption agent discharge port 209; Communicate by means of only the arm of described distribution house steward 210 and extraction thereof between described separate absorbent section 201 and degree of depth absorber portion 202; Separate absorbent section absorption agent discharge port 207 is provided with at the bottom of described rectifying tower; Described rectifying tower tower top is provided with MTBE gas phase discharge port 203; Described sulfide reboiled absorber column plate is located in rectifying tower, and described stage number N is: 5≤N≤50; The degree of depth absorber portion 202 on described sulfide reboiled absorber top and separate absorbent section 201 tower reactor of bottom are filled with dumped packing.
Embodiment 2
A method for MTBE sulfide contained by deep removal, as shown in Figure 1, its step is as follows:
With the integrated secondary reboiled absorber of embodiment 1 for sulfide reboiled absorber, sulphur content is the MTBE reboiled absorber separate absorbent section tower reactor pucking bubble charging of 620 μ g/g, MTBE volume pump flow is 200ml/h, reboiled absorber bottom temperature controls at 75 ~ 80 DEG C, METB mixture under thermogenic action with integrated secondary reboiled absorber 103 in the middle part of the methane amide liquid absorbent counter current contact that added by separate absorbent section absorption agent opening for feed 101, removing of most of sulfide is completed in separate absorbent section, the MTBE being stripped of most of sulfide enters the degree of depth absorber portion on integrated secondary reboiled absorber 103 top by the distribution house steward 210 in Fig. 2 and with the arm of dispersion pipe UNICOM bottom degree of depth absorber portion again, it is inner that methane amide absorption agent is imported degree of depth absorber portion by the absorption agent opening for feed in the middle part of degree of depth absorber portion, and submergence is arranged on the dispersion pipe bottom degree of depth absorber portion, divide sulfide in the MTBE shed after methane amide secondary deep absorbs by dispersion pipe in degree of depth absorber portion, qualified MTBE enters overhead condenser 104, tower top temperature is 52 ~ 56 DEG C, pressure is normal pressure, after overhead condenser 104 cools, temperature is that the MTBE of 40 ~ 50 DEG C enters return tank 105, reflux pump 107 is entered through return tank outlet pipe 106, act on next section MTBE at reflux pump 107 and enter integrated secondary reboiled absorber 103 through return line 110, another part MTBE enters products pot through MTBE products export pipe 111, reflux ratio is 5, the absorption agent of sulphur content 53080 μ g/g, from separate absorbent section absorption agent to be regenerated outlet pipe 108 and degree of depth absorber portion absorption agent outlet pipe 112 to be regenerated, 150ml altogether, enter absorbent regeneration tower 113, regenerator column bottom temperature is 230 ~ 240 DEG C, and tower top temperature is 120 ~ 150 DEG C, and pressure is normal pressure, the sulfide of removed overhead, through regenerator column overhead condenser 114, is delivered to sulfur recovery system by sulfide outlet pipe 115, after regeneration at the bottom of tower, absorption agent is after absorbent regeneration condenser 117, and the absorption agent opening for feed 101 entered in the middle part of integrated secondary reboiled absorber 103 recycles.
After regeneration, absorption agent sulphur content is 5000 μ g/g; MTBE sulphur content after desulfurization reaches 6 μ g/g, and mass yield is 99.93%.
Embodiment 3
A kind of method of MTBE sulfide contained by deep removal, overall flow is identical with embodiment 2, but difference is: the absorption agent 1. used is the mixture 200ml altogether of morpholine, methane amide, 2. 200ml θ ring filler is added at tower bottom of rectifying tower, 3. MTBE sulphur content is 850 μ g/g, and 4. reflux ratio is 0.2.
After the present embodiment regeneration, absorption agent sulphur content is 5000 μ g/g; MTBE sulphur content after desulfurization reaches 8 μ g/g, and mass yield is 99.91%.
Embodiment 4
A method for MTBE sulfide contained by deep removal, overall flow is identical with embodiment 2, but difference is: 1. MTBE sulphur content is 750 μ g/g, and 2. MTBE volume pump flow is 150ml/h; 3. reflux ratio is 10.
After the present embodiment regeneration, absorption agent sulphur content is 5000 μ g/g; MTBE sulphur content after desulfurization reaches 7 μ g/g, and mass yield is 99.92%.
Embodiment 5
A method for MTBE sulfide contained by deep removal, overall flow is identical with embodiment 2, but difference is: 1. MTBE sulphur content is 850 μ g/g, and 2. MTBE volume pump flow is 150ml/h; 3. regenerator column bottom temperature is 60 ~ 90 DEG C, and tower top temperature is 50 ~ 60 DEG C, and pressure is 25KPa (absolute pressure).
After the present embodiment regeneration, absorption agent sulphur content is 4800 μ g/g; MTBE sulphur content after desulfurization reaches 7 μ g/g, and mass yield is 99.90%.
Claims (9)
1. the method for a deep removal MTBE medium sulphide content, comprise the following steps: the methyl tertiary butyl ether MTBE of sulfur-bearing enters tower reactor from sulfide absorption distillation tower bottom, from bottom to top through being located at the separate absorbent section of rectifying tower bottom and being located at the degree of depth absorber portion of rectifier after heating; Through separate absorbent section, the MTBE mixture of gasification completes absorption with the liquid phase sulfide absorption agent counter current contact introducing rectifying tower separate absorbent section; Through degree of depth absorber portion, the MTBE mixture of gasification is dispersed to liquid absorbent inside, completes absorption by gas-liquid two-phase deep contact, the absorption agent of the sulfide that has finally been absorbed and the MTBE product through deep desulfuration; Described sulfide reboiled absorber is integral type double absorption rectifying tower, and its structure is divided at the bottom of tower from bottom to top, separate absorbent section (201), degree of depth absorber portion (202) and tower top; Described separate absorbent section (201) bottom column wall is provided with the sulfur-bearing MTBE opening for feed (206) be connected with the dispersion pipe in tower reactor, and separate absorbent section (201) middle part tower wall is provided with separate absorbent section absorption agent opening for feed (205); The distribution house steward (210) of top closure is provided with in described degree of depth absorber portion (202), this distribution house steward (210) lower ending opening is in separate absorbent section (201) top and to project up degree of depth absorber portion (202) inner, draws one or more arm communicate with the dispersion pipe bottom degree of depth absorber portion (202) from described distribution house steward (210); Described degree of depth absorber portion (202) middle part tower wall is provided with degree of depth absorber portion absorption agent opening for feed (204), and described degree of depth absorber portion (202) bottom column wall is provided with degree of depth absorber portion absorption agent discharge port (209); Communicate by means of only the arm of described distribution house steward (210) and extraction thereof between described separate absorbent section (201) and degree of depth absorber portion (202); Described separate absorbent section (201) top drum wall is provided with phegma mouth (208); Separate absorbent section absorption agent discharge port (207) is provided with at the bottom of described rectifying tower; Described rectifying tower tower top is provided with MTBE gas phase discharge port (203).
2. method according to claim 1, it is characterized in that: described method comprises further discharges from the bottom of described separate absorbent section and degree of depth absorber portion respectively by the absorption agent absorbing sulfide obtained in described sulfide reboiled absorber, enter absorbent regeneration tower, after regenerator column process, the sulfide that reclaiming tower top obtains, returns the absorbent regeneration obtained at the bottom of recovery tower to sulfide reboiled absorber simultaneously and recycles.
3. method according to claim 1, it is characterized in that: described method comprise further by obtain in described sulfide reboiled absorber through deep desulfuration MTBE product through cooling after, part MTBE backflow enters described sulfide reboiled absorber, another part MTBE is through MTBE product introduction products pot, and reflux ratio is: 0.2 ~ 10.
4. method according to claim 1, is characterized in that: described dispersion pipe adopts calandria or annular tube type; The degree of depth absorber portion (202) on described sulfide reboiled absorber top and separate absorbent section (201) tower reactor of bottom also load dumped packing further.
5. any one method described in claims 1 to 3, 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 acetyl morphine.
6. any one method described in claims 1 to 3, is characterized in that: absorption agent add-on and the MTBE inlet amount mass ratio of described separate absorbent section are 0.5 ~ 3:1.
7. any one method described in claims 1 to 3, is characterized in that: described sulfur-bearing MTBE enters reboiled absorber and the form of gas phase, liquid phase or gas-liquid mixed phase can be adopted to disperse charging from tower reactor.
8. method according to claim 1, it is characterized in that: the methyl tertiary butyl ether of sulfur-bearing enters the separate absorbent section tower reactor of described integrated secondary reboiled absorber from MTBE opening for feed, feed pressure is 0.1 ~ 1.5MPa, feeding temperature is 40 ~ 150 DEG C, tower reactor control temperature 65 ~ 90 DEG C, METB mixture under thermogenic action with integrated secondary reboiled absorber in the middle part of the liquid absorbent counter current contact that added by separate absorbent section absorption agent opening for feed, removing of most of sulfide is completed in separate absorbent section, the MTBE removing most of sulfide enters the degree of depth absorber portion on integrated secondary reboiled absorber top by distribution house steward and with the arm of dispersion pipe UNICOM bottom degree of depth absorber portion again, it is inner that absorption agent is imported degree of depth absorber portion by the absorption agent opening for feed in the middle part of degree of depth absorber portion, and submergence is arranged on the dispersion pipe bottom degree of depth absorber portion, divide sulfide in the MTBE shed after absorption agent secondary deep absorbs by dispersion pipe in degree of depth absorber portion, qualified MTBE enters overhead condenser, tower top control temperature is 50 ~ 60 DEG C, pressure is normal pressure, after overhead condenser cooling, temperature is that the MTBE of 40 ~ 50 DEG C enters return tank, reflux pump is entered through return tank outlet pipe, integrated secondary reboiled absorber is entered through return line at reflux pump effect next section MTBE, another part MTBE enters products pot through MTBE products export pipe, reflux ratio is 0.2 ~ 10, bottom sulfur absorbing agent automatic integral double absorption tower bottom of rectifying tower and tower top degree of depth absorber portion, absorbent regeneration tower is entered through separate absorbent section absorption agent to be regenerated outlet pipe and degree of depth absorber portion absorption agent outlet pipe to be regenerated, during regenerator column normal pressure: bottom temperature is 200 ~ 250 DEG C, tower top temperature is 90 ~ 160 DEG C, during decompression: bottom temperature is 60 ~ 90 DEG C, tower top temperature is 50 ~ 60 DEG C, and the sulfide of removed overhead, through regenerator column overhead condenser, is delivered to sulfur recovery system by sulfide outlet pipe, after regeneration at the bottom of tower, absorption agent is after absorbent regeneration condenser, and the absorption agent opening for feed entered in the middle part of integrated secondary reboiled absorber recycles.
9., for a sulfide reboiled absorber for the method for deep removal MTBE medium sulphide content according to claim 1, its structure is divided at the bottom of tower from bottom to top, separate absorbent section (201), degree of depth absorber portion (202) and tower top; Described separate absorbent section (201) bottom column wall is provided with the sulfur-bearing MTBE opening for feed (206) be connected with the dispersion pipe in tower reactor, and separate absorbent section (201) middle part tower wall is provided with separate absorbent section absorption agent opening for feed (205); The distribution house steward (210) of top closure is provided with in described degree of depth absorber portion (202), this distribution house steward (210) lower ending opening is in separate absorbent section (201) top and to project up degree of depth absorber portion (202) inner, draws one or more arm communicate with the dispersion pipe bottom degree of depth absorber portion (202) from described distribution house steward (210); Described degree of depth absorber portion (202) middle part tower wall is provided with degree of depth absorber portion absorption agent opening for feed (204), and described degree of depth absorber portion (202) bottom column wall is provided with degree of depth absorber portion absorption agent discharge port (209); Communicate by means of only the arm of described distribution house steward (210) and extraction thereof between described separate absorbent section (201) and degree of depth absorber portion (202); Separate absorbent section absorption agent discharge port (207) is provided with at the bottom of described rectifying tower; Described rectifying tower tower top is provided with MTBE gas phase discharge port (203).
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CN103524310B (en) * | 2013-10-16 | 2015-05-06 | 凯瑞化工股份有限公司 | Deep desulfurization method of MTBE (Methyl Tert-Butyl Ether) |
CN104262116A (en) * | 2014-06-23 | 2015-01-07 | 贺立明 | MTBE deep desulfurization device and method thereof |
CN104829436B (en) * | 2015-05-12 | 2016-08-17 | 中建安装工程有限公司 | The device and method of organic sulfur compound in a kind of deep removal methyl tertiary butyl ether(MTBE) |
CN106278834B (en) * | 2016-08-12 | 2018-09-18 | 丹东明珠特种树脂有限公司 | A kind of green MTBE deep desulfuration purifications agent and its in removing methyl tertiary butyl ether(MTBE) sulfide application |
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 |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN87100934A (en) * | 1986-02-26 | 1987-11-18 | 德国泰克萨科股份公司 | The method of continous seperating water from organic admixture |
US4847430A (en) * | 1988-03-21 | 1989-07-11 | Institut Francais Du Petrole | Process for manufacturing a tertiary alkyl ether by reactive distillation |
CN102898286A (en) * | 2012-08-21 | 2013-01-30 | 九江齐鑫化工有限公司 | Method for removing sulfides in MTBE by adsorptive distillation |
-
2013
- 2013-07-17 CN CN201310300138.9A patent/CN103333056B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN87100934A (en) * | 1986-02-26 | 1987-11-18 | 德国泰克萨科股份公司 | The method of continous seperating water from organic admixture |
US4847430A (en) * | 1988-03-21 | 1989-07-11 | Institut Francais Du Petrole | Process for manufacturing a tertiary alkyl ether by reactive distillation |
CN102898286A (en) * | 2012-08-21 | 2013-01-30 | 九江齐鑫化工有限公司 | Method for removing sulfides in MTBE by adsorptive distillation |
Non-Patent Citations (1)
Title |
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MTBE 深度脱硫技术的应用;张健民等;《化工进展》;20130630;第32卷(第6期);1453-1456 * |
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