CN1261396C - Method for preparing methyl alcohol in high purity - Google Patents
Method for preparing methyl alcohol in high purity Download PDFInfo
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- CN1261396C CN1261396C CN 03151148 CN03151148A CN1261396C CN 1261396 C CN1261396 C CN 1261396C CN 03151148 CN03151148 CN 03151148 CN 03151148 A CN03151148 A CN 03151148A CN 1261396 C CN1261396 C CN 1261396C
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- methyl alcohol
- methanol
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Abstract
The present invention relates to a method for preparing high-purity methanol, which comprises the following steps: orderly putting coarse methanol into a prerectifying tower, a pressurizing tower and a composite atmospheric tower to be rectified; respectively obtaining refining purified methanol from the tower top of the pressurizing tower and the tower top of the composite atmospheric tower. By the method of the present invention, synthesis methanol of which the purity is 95.50(wt%) can be refined into the high purity methanol, and the quality of the high-purity methanol conforms to the index set by Q/SWOQ1-2003. The present invention has the advantage of simple process and has a wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of methyl alcohol, relate in particular to a kind of process for purification of methyl alcohol, to obtain highly purified methyl alcohol.
Background technology
Methyl alcohol is a kind of important chemical industry raw material, in every field purposes is very widely arranged all.At present, 200,000 tons of methanol devices of general annual output, the synthetic gas that all adopts coal water slurry Texaco gasifier partial oxidation to be produced is a raw material, the thick methyl alcohol that is obtained carries out purification refine by four table flotation valve rectifying tower, equipment complexity not only, investment is big, and in the refining methyl alcohol that is obtained its ethanol content only accomplish＜100 * 10
-6, can not satisfy relevant field, especially the needs in field such as methyl chloride.
Summary of the invention
The technical issues that need to address of the present invention are the preparation methods that disclose a kind of high purity methanol, and to overcome the equipment complexity that prior art exists, investment is big, and the defective that the purity of the refining methyl alcohol that is obtained is low is to satisfy the needs of relevant department.
Method of the present invention comprises the steps:
Thick methyl alcohol is sent into the pre-rectifying tower, pressurizing tower and the compound atmospheric tower that are made of structured packing and trapezoidal guide float-valve tower tray successively and is carried out rectifying, is obtained the methyl alcohol of refining purifying respectively by pressurizing tower cat head and compound atmospheric tower cat head.
Preferable methods comprises the steps:
Synthetic next thick methyl alcohol is sent into the pre-rectifying tower middle part, remove in the thick methyl alcohol remaining gas dissolved therein and be the low-boiling-point substance of representative with the dme, the gas that the pre-rectifying tower cat head comes out is through cooling, be used as the pre-rectifying tower phegma under most of methanol steam condensation, the small portion non-condensable gas is gone into the non-condensable gas separator, is sent to other operation after isolating condensation methyl alcohol;
By the methyl alcohol that comes out at the bottom of the pre-rectifying tower tower, in interchanger, enter the pressurizing tower middle part after the heat exchange with pressurizing tower bottoms material, pressurizing tower cat head methanol steam enters condenser condenses, condensed methyl alcohol enters reboiler, with the heat exchange of compound atmospheric tower bottoms material, for compound atmospheric tower provides heat, the methanol solution part after the heat exchange is as the pressurizing tower phegma, and rest part is delivered to the refined methanol scale tank as product;
The methanol solution of discharging at the bottom of the pressurization Tata is delivered to compound atmospheric tower middle part after the interchanger heat exchange, the methanol steam that compound atmospheric tower cat head comes out is after cooling, a part is delivered to compound atmospheric tower top and is made phegma, rest part is after compound atmospheric tower refined methanol water cooler cooling, deliver to the refined methanol scale tank as product, provide heat by pressurizing tower cat head methanol steam condensation latent heat at the bottom of the compound normal pressure Tata.
Term " compound atmospheric tower " refers to: the tower inner member is combined by the corrugated plate regular packing and the trapezoidal guide float-valve tower tray of routine.Wherein, the top of tower is corrugated plate regular packing, and the bottom is trapezoidal guide float-valve tower tray.
Adopting method of the present invention, can be that the refining synthetic methanol of 95.50 (wt%) is to have the refining methyl alcohol shown in the table 1 with purity.The data of table 1 all adopt the method for Q/SWOQ1-2003 regulation to detect.
Table 1
| Project | Index |
| Colourity (platinum-cobalt), number | ≤5 |
| Density (20 ℃), g/cm3 | 0.7910-0.7916 |
| Boiling range, ℃ (101325Pa in 64.0～65.5 ℃ of scopes, comprises 64.6 ± 0.1 ℃), | ≤0.8 |
| The potassium permanganate test, min | ≥50 |
| Soluble test | Clarification |
| Moisture content, % | ≤0.10 |
| Acidity (in HCOOH), % or basicity are (with NH 3Meter), % | ≤0.0015 ≤0.0002 |
| Carbonyl compound content is (with CH 2The O meter), % | ≤0.002 |
| Residue on evaporation content, % | ≤0.001 |
| Sulfuric acid scrubbing test (but carbide) color, (platinum-cobalt) colourity | ≤50 |
| Ethanol content, % | ≤0.0050 |
| Iron (soluble) content, % | ≤0.000015 |
| Smell | The noresidue smell |
| Chloride ion content, % | ≤0.0001 |
This shows that method of the present invention compared with prior art has obvious improvement, not only invest for a short time, and can obtain the methyl alcohol of higher degree, can satisfy the needs of relevant department.
Description of drawings
Fig. 1 is a schema of the present invention.
Embodiment
Referring to Fig. 1, method of the present invention comprises the steps:
Synthetic next thick methyl alcohol is sent into pre-rectifying tower 1 middle part, the gas that the pre-rectifying tower cat head comes out is through cooling, be used as pre-rectifying tower 1 phegma under most of methanol steam condensation, the small portion non-condensable gas is gone into the non-condensable gas separator, is sent to other operation after isolating condensation methyl alcohol; Tower top temperature is 70～75 ℃, preferred 73 ℃;
By the methyl alcohol that comes out at the bottom of pre-rectifying tower 1 tower, in interchanger 3, enter pressurizing tower 2 middle parts after the heat exchange with pressurizing tower 2 bottoms material, pressurizing tower 2 cat head methanol steams enter condenser 4 condensations, condensed methyl alcohol enters reboiler 5, with compound atmospheric tower 6 bottoms material heat exchange, for compound atmospheric tower 6 provides heat, the methanol solution part after the heat exchange is as pressurizing tower 2 phegmas, and rest part is as product; Tower top temperature is 113～119 ℃, and reflux ratio is 2.7～2.8;
The methanol solution of discharging at the bottom of pressurizing tower 2 towers is delivered to compound atmospheric tower 6 middle parts after interchanger 3 heat exchange, the methanol steam that compound atmospheric tower 6 cats head come out is after cooling, a part is delivered to compound atmospheric tower 6 tops and is made phegma, rest part is after compound atmospheric tower 6 water coolers cooling, as product, provide heat by pressurizing tower 2 cat head methanol steam condensation latent heat at the bottom of compound atmospheric tower 6 towers.Tower top temperature is 64～68 ℃, and reflux ratio is 1.76～1.96.
Embodiment 1
Device parameter:
Pre-rectifying tower: φ 2400 * 26790mm, 33.7 meters of tower height overalls, in establish corrugated plate packing 7, highly be 10.7 meters.
Pressurizing tower: φ 2000 * 45340mm, 51.4 meters of tower height overalls, in establish corrugated plate packing 7, highly be 36 meters.
Compound atmospheric tower: φ 3000 * 47020mm, 53.1 meters of tower height overalls, corrugated plate packing 7 is arranged on top, highly is 21.1 meters, and trapezoidal guide float-valve tower tray 8 is arranged on the bottom.
Operating parameters sees Table 2.
| The logistics title | Thick methyl alcohol | The pressurizing tower charging | Pressurizing tower refluxes | Compound atmospheric tower charging | The pressurizing tower refined methanol | Compound atmospheric tower refluxes | Compound atmospheric tower refined methanol |
| Methyl alcohol (wt%) | 95.50 | 90.60 | 99.99 | 83.71 | 99.99 | 100 | 100 |
| Water | 3.54 | 9.32 | 16.15 | ||||
| Acetone | 20ppm | 8ppm | 17ppm | 2ppm | 17ppm | 2ppm | 2ppm |
| Ethanol | 250ppm | 239ppm | 9ppm | 407ppm | 9ppm | 9ppm | 9ppm |
| Fusel | 590ppm | 553ppm | 991ppm | ||||
| Light fraction | 0.874 | ||||||
| Flow kg/h | 46500 | 48709 | 56453 | 28108 | 20600 | 46972 | 23300 |
Its quality index reaches the data of table 1.
Claims (1)
1. the preparation method of a high purity methanol is characterized in that, comprises the steps:
Thick methyl alcohol is sent into the pre-rectifying tower (1), pressurizing tower (2) and the compound atmospheric tower (6) that are filled with structured packing successively and is carried out rectifying, is obtained the methyl alcohol of refining purifying respectively by pressurizing tower (2) cat head and compound atmospheric tower (6) cat head;
Thick methyl alcohol is sent into pre-rectifying tower (1) middle part, and the gas that the pre-rectifying tower cat head comes out is used as pre-rectifying tower (1) phegma through cooling under most of methanol steam condensation;
By the methyl alcohol that comes out at the bottom of pre-rectifying tower (1) tower, in interchanger (3), enter pressurizing tower (2) middle part after the heat exchange with pressurizing tower (2) bottoms material, pressurizing tower (2) cat head methanol steam enters condenser (4) condensation, condensed methyl alcohol enters reboiler (5), with the heat exchange of compound atmospheric tower (6) bottoms material, methanol solution part after the heat exchange is as pressurizing tower (2) phegma, and rest part is as product;
The methanol solution of discharging at the bottom of pressurizing tower (2) tower is delivered to compound atmospheric tower (6) middle part after interchanger (3) heat exchange, the methanol steam that compound atmospheric tower (6) cat head comes out is after cooling, a part is delivered to compound atmospheric tower (6) top and is made phegma, rest part is after the cooling of compound atmospheric tower (6) water cooler, as product;
Pre-rectifying tower (1) tower top temperature is 70～75 ℃;
Pressurizing tower (2) reflux ratio is 2.7～2.8;
Compound atmospheric tower (6) reflux ratio is 1.76～1.96;
Said compound normal pressure Tata inner member is combined by corrugated plate regular packing (7) and trapezoidal guide float-valve tower tray (8), and the top of tower is corrugated plate regular packing (7), and the bottom is a trapezoidal guide float-valve tower tray (8).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151148 CN1261396C (en) | 2003-09-23 | 2003-09-23 | Method for preparing methyl alcohol in high purity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03151148 CN1261396C (en) | 2003-09-23 | 2003-09-23 | Method for preparing methyl alcohol in high purity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1600762A CN1600762A (en) | 2005-03-30 |
| CN1261396C true CN1261396C (en) | 2006-06-28 |
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ID=34659863
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03151148 Expired - Lifetime CN1261396C (en) | 2003-09-23 | 2003-09-23 | Method for preparing methyl alcohol in high purity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1261396C (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1317248C (en) * | 2005-10-27 | 2007-05-23 | 天津大学 | Energy saving equipment of double effect rectification for methanol, and method |
| CN1328232C (en) * | 2006-03-10 | 2007-07-25 | 天津大学 | Double-efficient energy-saving and water-saving rectifying system and process for methanol |
| CN100378051C (en) * | 2006-06-13 | 2008-04-02 | 天津大学 | Rectifying tech. and equipment of high purity methanol |
| CN101130484B (en) * | 2007-09-07 | 2010-12-22 | 中国寰球工程公司 | Pressure-reducing flow-reversing dual-purpose distillation method and apparatus for refining crude methanol |
| CN102060661B (en) * | 2009-11-11 | 2013-04-10 | 兖矿国泰化工有限公司 | Process for operating methanol rectification system |
| CN102886151B (en) * | 2012-10-08 | 2014-12-17 | 安徽晋煤中能化工股份有限公司 | Device and method for recovering heat from three-tower methanol rectification |
| CN103342626B (en) * | 2013-07-31 | 2015-04-01 | 北京旭阳化工技术研究院有限公司 | Preparation method of chromatographic grade methanol |
| CN108558603B (en) * | 2018-06-06 | 2021-08-03 | 天津奥展兴达化工技术有限公司 | Three-tower three-effect crude methanol refining process method |
-
2003
- 2003-09-23 CN CN 03151148 patent/CN1261396C/en not_active Expired - Lifetime
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| Publication number | Publication date |
|---|---|
| CN1600762A (en) | 2005-03-30 |
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Owner name: SHANGHAI HUAYI ENERGY + CHEMICAL INDUSTRY CO., LTD Free format text: FORMER NAME: SHANGHAI COKING CO., LTD. |
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Address after: 200241 No. 4280 Wu Long Road, Shanghai Patentee after: SHANGHAI HUAYI ENERGY CHEMICAL CO.,LTD. Address before: 200241 No. 4280 Wu Long Road, Shanghai Patentee before: Shanghai Coking & Chemical Corp. |
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Granted publication date: 20060628 |