CN101898963A - Method for separating methyl acetate-methanol-water by adopting extractive distillation separation method with two-solvent lateral feed - Google Patents
Method for separating methyl acetate-methanol-water by adopting extractive distillation separation method with two-solvent lateral feed Download PDFInfo
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- CN101898963A CN101898963A CN2010101672883A CN201010167288A CN101898963A CN 101898963 A CN101898963 A CN 101898963A CN 2010101672883 A CN2010101672883 A CN 2010101672883A CN 201010167288 A CN201010167288 A CN 201010167288A CN 101898963 A CN101898963 A CN 101898963A
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Abstract
The invention relates to a method for separating methyl acetate-methanol-water by adopting an extractive distillation separation method with two-solvent lateral feed. The method comprises the following steps of: (1) carrying out two-solvent lateral feed on a methyl acetate, methanol and water mixed solution, carrying out extraction and separation with an extraction agent to obtain the methyl acetate with the mass content of more than 99.8 percent at the tower top, and controlling the temperature at the tower top to be 57.5 to 58.0 DEG C; (2) treating a mixing solution which contains the extraction agent and flows from a tower kettle through a regeneration tower and obtaining the methanol with the mass content of 95 percent at the tower top of the regeneration tower; (3) returning remaining distilling components to use; and (4) circularly using the extraction agent. The extraction agent adopts S2 water and S1 glycerol or ethylene glycol, wherein S1: S2 is equal to 0.5 to 1: 1. Compared with the traditional process, the invention has simple process, convenient recovery of the extraction agent, circular utilization and low energy consumption. The invention can obtain more than 99.8 percent of methyl acetate once with the yield of more than 95 percent and simultaneously obtain more than 95 percent of methanol.
Description
Technical field
The present invention relates to a kind of two strands of solvent side line extraction rectification techniques, be specifically related to a kind of two bursts of side entry feed extracting rectifying separating methyl acetate and methanol-aqueous systems, particularly a kind of method of two strands of solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water, and the employed equipment of this method.
Background technology
Ritalin is important chemical material and solvent, be widely used as the solvent of nitrocotton, cellulose acetate, camphor, grease, cured, gummy, various natural resins, in the Chemicals production process, raw material mainly as aceticanhydride, spices, medicine and fuel, make ethanamide and dimethylformamide product with ammonia or dimethylamine reaction, carry out transesterify with alcohol and produce a series of acetic esters, as the solvent and the spices of top grade.At present, China produces ritalin large and medium-sized enterprise and reaches family more than 20, about 290000 tons of year product, and along with the development of auxiliary agent, medicine and pharmaceutical industry, ritalin does not still satisfy the market requirement.China still introduced a large amount of ritalins from foreign country in 2008.According to the market situation analysis, the ritalin series product still had market preferably in 2010～2015 years.Ritalin can be made by esterification process, methyl alcohol hydroxylation method and acid anhydrides and methyl alcohol reaction method, also contains a large amount of acetic acid first vinegar in the waste liquid that produces in polyvinyl alcohol (PVC) Industrial processes.No matter esterification, or polyvinyl alcohol by product generates product and is ritalin, methyl alcohol, water mixed solution, and in the above-mentioned mixing solutions, ritalin, methyl alcohol, water form binary, ternary azeotrope, adopts rectifying to be difficult to separate between the composition.Traditional industry adopts and adds the water azeotrope that the formation of water azeotropic distillation contains ritalin 96.5% (wt%), adopt siccative then or generate crystalline alkali and salt compounds dehydration with water, can get the ritalin more than 99.5%, this process is complicated, alkali and salt recycle process energy consumption height, discharge of wastewater is bigger.
Summary of the invention
The present invention will provide a kind of method of a kind of two strands of solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water newly, and the employed equipment of this method, compare with traditional technology, the novel method processing step is fairly simple, extraction agent is convenient to reclaim, recycle, and energy consumption is low.The present invention adopts two bursts of side entry feed extraction process separating acetic acid methyl esters-methyl alcohol-aqueous systems, and stock liquid can once obtain the ritalin more than 99.8% after two bursts of side entry feed extractions, yield can reach more than 95%, obtain 95% above methyl alcohol simultaneously, this technological process is simple, and energy consumption is low.
The scheme of finishing the foregoing invention task is that a kind of method of two strands of solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water is characterized in that step is as follows:
(1), ritalin, methyl alcohol, water mixed liquid be through two bursts of side entry feed, the extraction agent extracting and separating, cat head gets the ritalin of mass content more than 99.8%, tower top temperature is controlled at 57.5～58.0 ℃;
(2), the tower still flows out the mixed solution contain extraction agent and handles through regenerator column, the regenerator column cat head gets mass content 95% methyl alcohol;
(3), all the other cuts are returned and are used;
(4), extraction agent recycles.
Wherein, described extraction agent adopts S2 (water) and S1 (glycerine or ethylene glycol).S1∶S2＝0.5～1∶1。
More optimize and more particularly, the method for two strands of solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water of the present invention is one two bursts side entry feed extracting rectifying separating methyl acetate and methanol-aqueous systems, technology is as follows:
(1), behind the esterification reaction rectification or synthesizing polyethylene alcohol (PVC) by-product solution cut 1. enter two strands of side entry feed extraction towers, the control tower top temperature is at 57.5～58.0 ℃, NS2, the charging of NS1 position above raw material respectively of extraction agent S2 water (cut 3.) and extraction agent S1 (cut 4.) glycerine (or ethylene glycol), cat head are the ritalin (cut 2.) more than 99.8%; (2), two strands of side entry feed extraction tower still mixed solutions handle through regenerator column, regeneration overhead distillates cut respectively, is respectively 6. 7. (95.5% methyl alcohol), cut 8. (water and Trace Methanol) of (96～97% ritalins, methyl alcohol), cut of cut;
(3), 1. 6. cut be returned to cut, 7. cut is 95% above methyl alcohol, 3. 8. cut deliver to cut;
(4), the after cut of regenerator column bottom reason 5. (solvent) deliver to cut and 3. recycle.
More particularly: ritalin, methyl alcohol and water mixed solution (cut 1.): ritalin 80%, water 3%, methyl alcohol 17%) enter two strands of side entry feed extraction towers, the control tower top temperature is at 57.5～58.0 ℃, cat head is the ritalin more than 99.8%, NS2, the charging of NS1 position above raw material respectively of extraction agent S2 water and extraction agent S1 glycerine.Two strands of side entry feed extraction tower still mixed solutions are handled through regenerator column, regeneration overhead distillates 6. 7. (95.5% methyl alcohol), cut 8. (water and Trace Methanol) of (96～97% ritalins, methyl alcohol), cut of cut respectively, 1. 6. cut be returned to cut, 7. cut is 95% above methyl alcohol, 3. 8. cut deliver to cut, and 5. reason back, regenerator column bottom solvent is delivered to cut and 3. recycled.The processing condition of sepn process: each tower still temperature control, reflux ratio, feed entrance point and stage number are shown in Table 1 in the sepn process.
Table 1 sepn process processing condition
| Number of theoretical plate (N) | 57? | 21? |
| Raw material feed entrance point (NF) | 49? | 11? |
| Extractant feed position (NS 1) | 6? | /? |
| Extractant feed position (NS2) | 24? | /? |
The present invention compares with traditional technology, and processing step is simple, and extraction agent is convenient to reclaim, recycle, and energy consumption is low.The present invention can once obtain the ritalin more than 99.8%, and yield can reach more than 95%, obtains 95% above methyl alcohol simultaneously.
Description of drawings
Fig. 1 is the process flow sheet of two bursts of side entry feed extracting and separating methyl acetate and methanol-aqueous systems;
Fig. 2 is two strands of side entry feed extraction experiments devices;
Fig. 3, Fig. 4 are respectively the measurement result figure of two strands of side entry feed extraction plants, solvent reclamation device;
Fig. 5 is the process flow sheet of rectifying with the integrated separating methyl acetate and methanol system of extraction.
Embodiment
1: two strand of side entry feed extraction process of embodiment and experimental installation see figures.1.and.2 respectively, and 7 is feed sump among Fig. 2, and 8 is pump, and 9 is glass rotameter, 10 is storage tank, and 11 is electric mantle, and 12 is the tower still, and 13 is tower still thermometer, 14 storage tanks, 15 is pump, 16 storage tanks, 17 is pump, and 18,19 is glass rotameter, and 20 is glass fibre cotton and chuck, 21 is filler, and 22 is return line, and 23 is refluxing opening, 24 is the tower top temperature meter, and 25 is condenser, 26 electromagnetic wands.Methyl acetate and methanol-water mixed liquid that sub-petro-chemical corporation is raised in employing to be provided is a raw material, analyzes through the HP chromatographic instrument, forms and sees among Fig. 3, forms among the figure to be mass content.Stock liquid is through two bursts of side entry feed extraction tower extracting and separating, and tower top temperature is 57.5～58.0 ℃, can get the ritalin more than 99.8%, and the ritalin yield reaches more than 95.5%, is the aqueous glycerin solution that contains 0.1% left and right sides ritalin at the bottom of the tower.Experiment is carried out under normal pressure, and the tower internal diameter is 22mm, interior dress
The Stainless Steel Helices of 3*3 θ type is through measuring this height equivalent to one theoretical plate HETP=27mm with standards system.The tower still heats with electric mantle, all with the glass rotameter metering, trim the top of column is regulated with electromagnetic wand for overhead product discharging and raw material, solvent, charging, and the tower still is extracted out with vacuum pump, composition is seen shown in Figure 3 at the bottom of the tower, the tower bottom flow fluid is returned to solvent regeneration tower, and the regenerator column operational condition is as shown in table 1, and solvent recycles after taking off ester, dealcoholysis, dehydration, after regenerator column is handled, form as shown in Figure 4 at the bottom of cat head, the tower, cat head can get 95% methyl alcohol, and other cut all can be recycled.
Claims (4)
1. the method for one kind two strands solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water is characterized in that step is as follows:
(1), ritalin, methyl alcohol, water mixed liquid be through two bursts of side entry feed, the extraction agent extracting and separating, cat head gets the ritalin of mass content more than 99.8%, tower top temperature is controlled at 57.5～58.0 ℃;
(2), the tower still flows out the mixed solution contain extraction agent and handles through regenerator column, the regenerator column cat head gets mass content 95% methyl alcohol;
(3), all the other cuts are returned and are used;
(4), extraction agent recycles.
2. according to the method for the described two strands of solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water of claim 1, it is characterized in that described extraction agent adopts S2 water and S1 glycerine or ethylene glycol; S1: S2=0.5～1: 1.
3. according to the method for the described two strands of solvent side entry feed extracting rectifying partition method separating methyl acetate and methanol-water of claim 1, it is characterized in that the concrete operations of described each step are:
Ritalin, methyl alcohol and water mixed solution be cut 1.: wherein ritalin 80%, water 3%, methyl alcohol 17%; Enter two strands of side entry feed extraction towers;
2. the cut of cat head is the ritalin more than 99.8%, and cut 3. extraction agent S2 is a water, and cut 4. extraction agent S1 be glycerine, NS2, the charging of NS1 position above raw material respectively; Two strands of side entry feed extraction tower still mixed solutions are handled through regenerator column, regeneration overhead distillate respectively cut 6., cut 7. with cut 8.; 6. this cut is 96～97% ritalins, methyl alcohol; 7. this cut is 95.5% methyl alcohol; 8. this cut is water and Trace Methanol; 1. 6. cut be returned to cut, and 3. 8. cut deliver to cut, and 5. reason back, regenerator column bottom solvent is delivered to cut and 4. recycled.
4. according to two strands of side entry feed extraction and rectification separation methods of claim 1 or 2 or 3 described ritalins, it is characterized in that, processing parameter in described each step is as follows: 81～85 ℃ of two strands of side entry feed extraction tower column bottom temperatures, reflux ratio 3～4,57～100 ℃ of regenerator column tower top temperatures, 202 ℃ of column bottom temperatures, reflux ratio 1～3.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120719A (en) * | 2010-08-26 | 2011-07-13 | 江苏沿江化工资源开发研究院有限公司 | Method for separating methyl acetate, methanol and water through two-trickle solvent side charging extractive distillation separating method and device thereof |
| CN102180791A (en) * | 2011-04-13 | 2011-09-14 | 天津大学 | Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification |
| CN102863333A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Method for extracting high purity methyl acetate in methyl acetate-methanol-water mixed liquor |
| CN102863334A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Method for preparing high purity methyl acetate by adding salt, extracting and rectifying |
| CN102924275A (en) * | 2012-11-27 | 2013-02-13 | 福州大学 | Refining method for alcoholysis waste liquid in PVA (polyvinyl alcohol) production and test device for same |
| CN103755559A (en) * | 2014-01-08 | 2014-04-30 | 沈阳化工大学 | Method for separating ethyl acetate-isopropanol by ionic liquid extractive rectification |
| CN105439819A (en) * | 2014-08-27 | 2016-03-30 | 中国石油化工股份有限公司 | A separating process for ethanol production by methyl acetate hydrogenation |
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| US4543164A (en) * | 1983-04-14 | 1985-09-24 | Lloyd Berg | Separation of methyl acetate from methanol by extractive distillation |
| CN1526692A (en) * | 2003-09-22 | 2004-09-08 | ����ʦ����ѧ | Composite extracting and rectifying separation process of ethyl acetate |
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2010
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Patent Citations (2)
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| US4543164A (en) * | 1983-04-14 | 1985-09-24 | Lloyd Berg | Separation of methyl acetate from methanol by extractive distillation |
| CN1526692A (en) * | 2003-09-22 | 2004-09-08 | ����ʦ����ѧ | Composite extracting and rectifying separation process of ethyl acetate |
Non-Patent Citations (1)
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| 盖丽芳等: "高纯度醋酸甲酯精制新工艺", 《河北工业科技》, vol. 24, no. 1, 31 January 2007 (2007-01-31), pages 19 - 21 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102120719A (en) * | 2010-08-26 | 2011-07-13 | 江苏沿江化工资源开发研究院有限公司 | Method for separating methyl acetate, methanol and water through two-trickle solvent side charging extractive distillation separating method and device thereof |
| CN102180791A (en) * | 2011-04-13 | 2011-09-14 | 天津大学 | Method for separating methyl acetate-methanol mixture by ionic liquid intermittent extractive rectification |
| CN102863333A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Method for extracting high purity methyl acetate in methyl acetate-methanol-water mixed liquor |
| CN102863334A (en) * | 2011-07-04 | 2013-01-09 | 中国石油化工股份有限公司 | Method for preparing high purity methyl acetate by adding salt, extracting and rectifying |
| CN102863334B (en) * | 2011-07-04 | 2014-09-03 | 中国石油化工股份有限公司 | Method for preparing high purity methyl acetate by adding salt, extracting and rectifying |
| CN102863333B (en) * | 2011-07-04 | 2014-12-10 | 中国石油化工股份有限公司 | Method for extracting high purity methyl acetate in methyl acetate-methanol-water mixed liquor |
| CN102924275A (en) * | 2012-11-27 | 2013-02-13 | 福州大学 | Refining method for alcoholysis waste liquid in PVA (polyvinyl alcohol) production and test device for same |
| CN103755559A (en) * | 2014-01-08 | 2014-04-30 | 沈阳化工大学 | Method for separating ethyl acetate-isopropanol by ionic liquid extractive rectification |
| CN103755559B (en) * | 2014-01-08 | 2016-04-06 | 沈阳化工大学 | A kind of method of ion liquid abstraction rectifying separation ethyl acetate-isopropanol |
| CN105439819A (en) * | 2014-08-27 | 2016-03-30 | 中国石油化工股份有限公司 | A separating process for ethanol production by methyl acetate hydrogenation |
| CN105439819B (en) * | 2014-08-27 | 2017-10-27 | 中国石油化工股份有限公司 | The separation method of methyl acetate preparation of ethanol by hydrogenating |
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Application publication date: 20101201 |