CN103242135A - Method and device for rectifying methanol - Google Patents
Method and device for rectifying methanol Download PDFInfo
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- CN103242135A CN103242135A CN2013102098762A CN201310209876A CN103242135A CN 103242135 A CN103242135 A CN 103242135A CN 2013102098762 A CN2013102098762 A CN 2013102098762A CN 201310209876 A CN201310209876 A CN 201310209876A CN 103242135 A CN103242135 A CN 103242135A
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Abstract
The invention discloses a method and a device for rectifying methanol. The method comprises: inputting crude methanol into a methanol pre-rectifying tower to be rectified, and adding alkali liquor in the crude methanol through the lower part of a stripping section of the methanol pre-rectifying tower when inputting the crude methanol into the methanol pre-rectifying tower. The methanol rectifying device comprises the methanol pre-rectifying tower and an alkali adding device, wherein the alkali adding device is communicated with the lower part of the stripping section of the methanol pre-rectifying tower. Since the alkali liquor is added in the crude methanol from the lower part of the stripping section of the methanol pre-rectifying tower in the technical scheme provided by the invention, the alkali liquor adding position is changed so as to quickly and stably adjust the acid value of refined methanol produced by a rectifying process to meet the standard.
Description
Technical field
The present invention relates to thick methanol rectification technical field, in particular to a kind of method and device of methanol rectification.
Background technology
Methanol rectifying system is to be raw material with thick methyl alcohol, produces the device of the refined methanol product that meets GB338-2004 and the O-M-232E of the United States Federal standard, and it is the terminal production equipment of methanol production enterprise.
It is synthetic that the thick methyl alcohol of the raw material of methanol rectification comes from methyl alcohol, is subjected to the influence of synthetic reaction condition, except methyl alcohol, water, also has CO in the thick methyl alcohol
2, various impurity such as acetone, ethanol, formic acid, acetic acid, make thick methanol product be slightly acidic.Therefore, when thick methyl alcohol is carried out rectifying, no matter adopt which kind of rectification process at present, all need adding concentration in thick methyl alcohol is 3%~5% sodium hydroxide lye, purpose is lower boiling and the high boiling point acids in the neutralized crude methyl alcohol, the equipment and the pipeline that prevent rectifying corrode, and can promote the decomposition of carbonyl compound in the thick methyl alcohol in addition, are conducive to rectifying.
At present, the methanol rectification production technique is used more general have three domestic towers or three-plus-one tower (advection) methanol rectification technology, external methanol rectification three towers (adverse current) technology as Topsoe.These two kinds of rectification process all can be produced the refined methanol product of the AA level that can reach GB338-2004 premium grads and u.s. federal standard O-M-232E.The acid number in the refined methanol (in HCOOH)≤0.00015% wherein.Before rectifying pre-rectifying tower that thick methyl alcohol is made a gift to someone, all design the sodium hydroxide lye that adds concentration 3~5% at the pan feeding pipeline of thick methyl alcohol, reach lower boiling and high boiling point acids in the neutralized crude methyl alcohol, prevent the equipment of rectifying and the purpose that corrosion takes place pipeline.
But, no matter be methanol rectification three towers (adverse current) technology of the Topsoe that adopts of domestic methanol rectifying system or domestic part producer, after rectifier unit came into operation, it was defective refined methanol product acidity all to occur, did not reach the problem of premium grads standard.
Summary of the invention
The present invention aims to provide a kind of method and device of methanol rectification, and is defective with refined methanol product acidity in the solution prior art, do not reach premium grads standard techniques problem.
To achieve these goals, according to an aspect of the present invention, provide a kind of method of methanol rectification.This method comprises the step that thick methyl alcohol input methyl alcohol pre-rectifying tower is carried out rectifying, and in the step of carrying out rectifying with thick methyl alcohol input methyl alcohol pre-rectifying tower, the bottom of the stripping section by the methyl alcohol pre-rectifying tower adds alkali lye in thick methyl alcohol.
Further, the methyl alcohol pre-rectifying tower is advection three-tower rectification tower, three-plus-one rectifying tower or adverse current three-tower rectification tower.
Further, the methyl alcohol pre-rectifying tower is tray column, and the stripping section by the tray column top position of the 15th block of arbitrary block of column plate below the column plate from bottom to top adds alkali lye.
Further, the methyl alcohol pre-rectifying tower is packing tower, and the top of the packing section of the hypomere by packing tower adds alkali lye.
Further, the temperature of alkali lye is 50~60 ℃ and to keep the pH value of methanol solution in the tower reactor of pre-rectifying tower be 7~9.
According to another aspect of the present invention, provide a kind of methanol rectifying system.This methanol rectifying system comprises the methyl alcohol pre-rectifying tower, also comprises adder-subtractor, and adder-subtractor is connected with the stripping section bottom of methyl alcohol pre-rectifying tower.
Further, the methyl alcohol pre-rectifying tower is advection three-tower rectification tower, three-plus-one rectifying tower or adverse current three-tower rectification tower.
Further, the methyl alcohol pre-rectifying tower is tray column, in the stripping section of adder-subtractor and methyl alcohol pre-rectifying tower from bottom to top the position of the following arbitrary column plate top of the 15th block of column plate be connected.
Further, adder-subtractor adds pipeline by alkali lye and is connected with the methyl alcohol pre-rectifying tower, and alkali lye adding pipeline is provided with steam companion thermic devices.
Further, alkali lye adding pipeline is provided with and adds the alkali volume pump.
The present inventor finds, the refined methanol product acidity that occurs after rectifier unit of the prior art comes into operation is defective, to cause rectifying refined methanol product not reach premium grads standard techniques problem be because the implantation site that adds of sodium hydroxide solution is all designed on thick methyl alcohol pan feeding pipeline, adds that the implantation site is unreasonable causes.Technical scheme of the present invention has changed the implantation site that adds of alkali lye owing to be that stripping section bottom by the methyl alcohol pre-rectifying tower adds alkali lye in thick methyl alcohol, thereby makes the acid number fast and stable in the refined methanol of rectification process production reach standard.
Description of drawings
The Figure of description that constitutes the application's a part is used to provide further understanding of the present invention, and illustrative examples of the present invention and explanation thereof are used for explaining the present invention, do not constitute improper restriction of the present invention.In the accompanying drawings:
Fig. 1 shows the local structure synoptic diagram of methanol rectifying system according to an embodiment of the invention; And
Fig. 2 shows the local structure synoptic diagram of methanol rectifying system according to another embodiment of the present invention.
Embodiment
Need to prove that under the situation of not conflicting, embodiment and the feature among the embodiment among the application can make up mutually.Describe the present invention below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
The present inventor finds, the refined methanol product acidity that occurs after rectifier unit of the prior art comes into operation is defective, to cause rectifying refined methanol product not reach premium grads standard techniques problem be because the implantation site that adds of sodium hydroxide solution is all designed on thick methyl alcohol pan feeding pipeline, adds that the implantation site is unreasonable causes.
A kind of typical embodiment according to the present invention provides a kind of method of methanol rectification.This method comprises the step that thick methyl alcohol input methyl alcohol pre-rectifying tower 10 is carried out rectifying, in the step of carrying out rectifying with thick methyl alcohol input methyl alcohol pre-rectifying tower 10, the stripping section bottom by methyl alcohol pre-rectifying tower 10 adds alkali lye (as shown in Figure 1, 2) in thick methyl alcohol.Technical scheme of the present invention has changed the implantation site that adds of alkali lye owing to be that stripping section bottom by methyl alcohol pre-rectifying tower 10 adds alkali lye in thick methyl alcohol, thereby makes the acid number fast and stable in the refined methanol of rectification process production reach standard.
The present invention is by this change, and it is as follows to make acid number fast and stable in the refined methanol of rectification process production reach the reason of standard:
Contain 3%~6% H in the synthetic thick methyl alcohol of producing
2O also contains CO simultaneously
2, impurity such as ethanol, propyl alcohol, formic acid, acetic acid.When concentration is after 3%~5% sodium hydroxide solution adds in the thick methyl alcohol, sodium hydroxide with thick methyl alcohol in formic acid and acetic acid generation neutralization reaction in, also and CO
2With H
2The weak acid that O the generates production sodium bicarbonate that reacts.Sodium bicarbonate is strong base-weak acid salt, and it can not decompose under the operating environment of pre-77 ℃ of (cat head)~84.5 of tower ℃ (at the bottom of the tower) fully, enters main distillation column with still liquid, and service temperature is higher in main rectifying, and carbonate decomposes again, discharges CO at cat head
2, enter in the refined methanol, cause refined methanol product acidity defective.For this reason; when in distillation system, adding alkali lye; must guarantee that alkali lye and acids in the thick methyl alcohol neutralize when playing the effect of protection rectifying device pipeline, also need guarantee in pre-tower methyl alcohol in the lower boiling acids get rid of fully, guarantee that rectifying product acidity is qualified.Therefore, of the present invention taking adds alkali lye from the higher column plate (filler) of the bottom stripping section temperature of tower, thereby the lower boiling acids is got rid of fully in guaranteeing in pre-tower methyl alcohol, has guaranteed that rectifying product acidity is qualified.
Preferably, methyl alcohol pre-rectifying tower 10 is advection three-tower rectification tower, three-plus-one rectifying tower or adverse current three-tower rectification tower.
Among the present invention the alkali lye of methyl alcohol pre-rectifying tower added the implantation site and transform stripping section bottom to the methyl alcohol pre-rectifying tower from thick methyl alcohol pan feeding pipeline 50.Specifically add the implantation site, can determine according to the detailed construction of methyl alcohol pre-rectifying tower.A kind of typical embodiment according to the present invention, the methyl alcohol pre-rectifying tower is tray column, the stripping section by the methyl alcohol pre-rectifying tower top position of the 15th block of arbitrary block of column plate below the column plate from bottom to top adds alkali lye.Certainly, be the pre-rectifying tower of filler for methyl alcohol pre-rectifying tower internals, the filler top that can be chosen in hypomere adds alkali lye.Preferably, alkali lye adds pipeline 40 by alkali lye and adds methyl alcohol pre-rectifying tower 10, and has steam companion heat in the alkali lye adition process.The alkali lye pipeline arranges steam tracing, can improve alkali liquid temperature on the one hand to improve the solubleness of sodium hydroxide in water, prevent its crystallization blocking pipeline, can prevent that on the other hand winter, alkali lye pipeline inner product liquid froze stifledly, guarantee that alkali lye measures in the normal adding tower on demand.The pH value of the interior methanol solution of the tower reactor of adding temperature, flow velocity and the pre-rectifying tower of alkali lye all can be realized in the scope that adopt usually this area among the present invention, preferably, the temperature of alkali lye is 50~60 ℃, and the pH value of methanol solution is 7~9 in the tower reactor of maintenance pre-rectifying tower.
A kind of typical embodiment provides a kind of methanol rectifying system according to the present invention.This methanol rectifying system comprises methyl alcohol pre-rectifying tower 10 and adder-subtractor 20, and adder-subtractor 20 is connected with the stripping section bottom of methyl alcohol pre-rectifying tower 10.Technical scheme of the present invention has changed the implantation site that adds of alkali lye owing to be that stripping section bottom by methyl alcohol pre-rectifying tower 10 adds alkali lye in thick methyl alcohol, thereby makes the acid number fast and stable in the refined methanol of rectification process production reach standard.Preferably, methyl alcohol pre-rectifying tower 10 is advection three-tower rectification tower, three-plus-one rectifying tower or adverse current three-tower rectification tower.
A kind of typical embodiment according to the present invention, methyl alcohol pre-rectifying tower 10 is tray column, the stripping section of adder-subtractor 20 and tray column is connected by the top position of the 15th block of arbitrary block of column plate below the column plate from bottom to top.Preferably, adder-subtractor 20 adds pipeline 40 by alkali lye and is connected with methyl alcohol pre-rectifying tower 10, and alkali lye adding pipeline 40 is provided with steam companion thermic devices.The alkali lye pipeline arranges steam tracing, can improve alkali liquid temperature on the one hand to improve the solubleness of sodium hydroxide in water, prevent its crystallization blocking pipeline, can prevent that on the other hand winter, alkali lye pipeline inner product liquid froze stifledly, guarantee that alkali lye measures in the normal adding tower on demand.
Preferably, alkali lye adding pipeline 40 is provided with and adds alkali volume pump 30, the convenient control that adds the alkali lye amount.Preferably, the material of alkali lye adding pipeline 40 is stainless steel.
Use technical scheme of the present invention, with the methyl alcohol pre-rectifying tower add the alkali pipeline from the pan feeding pipeline modification to the column plate of pre-tower bottom, the acidity of the refined methanol product of rectifier unit obviously descends, reached the standard of GB GB338-2004 premium grads, and product acidity is all the time below 10ppm, thereby guaranteed that the refined methanol product remains premium grads.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the method for a methanol rectification, comprise the step that thick methyl alcohol input methyl alcohol pre-rectifying tower (10) is carried out rectifying, it is characterized in that, described thick methyl alcohol is imported in the step of carrying out rectifying of described methyl alcohol pre-rectifying tower (10), the bottom of the stripping section by described methyl alcohol pre-rectifying tower (10) adds alkali lye in described thick methyl alcohol.
2. method according to claim 1 is characterized in that, described methyl alcohol pre-rectifying tower (10) is advection three-tower rectification tower, three-plus-one rectifying tower or adverse current three-tower rectification tower.
3. method according to claim 1 is characterized in that, described methyl alcohol pre-rectifying tower (10) is tray column, and the stripping section by described tray column adds described alkali lye in the top position of the 15th block of arbitrary block of column plate below the column plate from bottom to top.
4. method according to claim 1 is characterized in that, described methyl alcohol pre-rectifying tower (10) is packing tower, and the top of the packing section of the hypomere by described packing tower adds described alkali lye.
5. method according to claim 1 is characterized in that, the temperature of described alkali lye is 50~60 ℃, and to keep the pH value of methanol solution in the tower reactor of described pre-rectifying tower be 7~9.
6. a methanol rectifying system comprises the methyl alcohol pre-rectifying tower, it is characterized in that, also comprises adder-subtractor (20), and described adder-subtractor (20) is connected with the bottom of the stripping section of described methyl alcohol pre-rectifying tower (10).
7. methanol rectifying system according to claim 6 is characterized in that, described methyl alcohol pre-rectifying tower (10) is advection three-tower rectification tower, three-plus-one rectifying tower or adverse current three-tower rectification tower.
8. methanol rectifying system according to claim 6, it is characterized in that, described methyl alcohol pre-rectifying tower (10) is tray column, in the stripping section of described adder-subtractor (20) and described methyl alcohol pre-rectifying tower (10) from bottom to top the position of the following arbitrary column plate top of the 15th block of column plate be connected.
9. methanol rectifying system according to claim 8, it is characterized in that, described adder-subtractor (20) adds pipeline (40) by alkali lye and is connected with described methyl alcohol pre-rectifying tower (10), and described alkali lye adding pipeline (40) is provided with steam companion thermic devices.
10. methanol rectifying system according to claim 9 is characterized in that, described alkali lye adding pipeline (40) is provided with and adds alkali volume pump (30).
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CN2013102098762A CN103242135A (en) | 2013-05-30 | 2013-05-30 | Method and device for rectifying methanol |
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Cited By (1)
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CN103524301A (en) * | 2013-10-31 | 2014-01-22 | 神华集团有限责任公司 | Methyl alcohol rectification system and method for recycling methyl alcohol in incondensable gas of system |
Citations (3)
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CN202277823U (en) * | 2011-10-28 | 2012-06-20 | 陕西长青能源化工有限公司 | Alkaline adding device for producing methanol from coal |
CN102728090A (en) * | 2012-07-10 | 2012-10-17 | 东北制药集团股份有限公司 | Fractional distillation equipment for separating propargyl alcohol and method of equipment |
CN203281057U (en) * | 2013-05-30 | 2013-11-13 | 神华集团有限责任公司 | Methanol rectification apparatus |
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2013
- 2013-05-30 CN CN2013102098762A patent/CN103242135A/en active Pending
Patent Citations (3)
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CN202277823U (en) * | 2011-10-28 | 2012-06-20 | 陕西长青能源化工有限公司 | Alkaline adding device for producing methanol from coal |
CN102728090A (en) * | 2012-07-10 | 2012-10-17 | 东北制药集团股份有限公司 | Fractional distillation equipment for separating propargyl alcohol and method of equipment |
CN203281057U (en) * | 2013-05-30 | 2013-11-13 | 神华集团有限责任公司 | Methanol rectification apparatus |
Non-Patent Citations (1)
Title |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103524301A (en) * | 2013-10-31 | 2014-01-22 | 神华集团有限责任公司 | Methyl alcohol rectification system and method for recycling methyl alcohol in incondensable gas of system |
CN103524301B (en) * | 2013-10-31 | 2015-04-22 | 神华集团有限责任公司 | Methyl alcohol rectification system and method for recycling methyl alcohol in incondensable gas of system |
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Application publication date: 20130814 |