CN102633770A - Method and device for removing light components in trioxymethylene - Google Patents
Method and device for removing light components in trioxymethylene Download PDFInfo
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- CN102633770A CN102633770A CN2012100989791A CN201210098979A CN102633770A CN 102633770 A CN102633770 A CN 102633770A CN 2012100989791 A CN2012100989791 A CN 2012100989791A CN 201210098979 A CN201210098979 A CN 201210098979A CN 102633770 A CN102633770 A CN 102633770A
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Abstract
The invention discloses a method and a device for removing light components in trioxymethylene, which belong to the technical field of purification of trioxymethylene. The method includes the following steps of firstly, feeding extracted trioxymethylene, benzene and small amount of mixture of water and organic matter into a light component removing tower to remove light components, returning to extraction process after gas on the top of the light component removing tower is condensed and cooled; and secondly; feeding trioxymethylene at the bottom of the light component removing tower and small amount of mixture of water, methyl alcohol, formaldehyde, formic acid and the like to be stripped in a stripper. By adding the stripper, temperature at the bottom of the light component removing tower and backflow ratio can be reduced by the additional stripping process, energy consumption is reduced greatly, trioxymethylene can be prevented from being decomposed greatly, and purity of trioxymethylene can be improved effectively.
Description
Technical field
The present invention relates to trioxymethylene purification techniques field, especially a kind of trioxymethylene removes the method and the device of light constituent.
Background technology
Trioxymethylene is the important source material of production engineering plastics polyoxymethylene.Require trioxymethylene purity>=99.98% in the production process, water≤100ppm, other impurity (comprising that methyl alcohol, formaldehyde, formic acid, reorganization grade)≤100ppm.Trioxymethylene concentration after synthesizing, concentrating reaches 30%～50%; Because the mixture of trioxymethylene, formaldehyde, water can form trioxymethylene-formaldehyde-water ternary azeotropic component; Simple distillation technique is difficult to the purification trioxymethylene; Later separation is made with extra care and is mainly contained two kinds of methods, i.e. freeze crystallization and extraction separation method at present.Extraction process wherein; Be to adopt extraction agents such as benzene, ethylene dichloride that trioxymethylene is separated from water; Through lightness-removing column extraction agent and the lighter impurity of boiling point are separated then; The higher trioxymethylene solution of concentration is removed the boiling point impurity high than trioxymethylene through weight-removing column again, finally obtains the trioxymethylene of purity >=99.98%.But this kind method in process of production, and taking off the light industry preface, to remove the light component turndown ratio minimum, and Trace Methanol in the tower still trioxymethylene solution, formaldehyde, formic acid, water-content are higher; General trioxymethylene content is 99.90%～99.96%, and methanol content is 50～180ppm, and formaldehyde content is 60～210ppm; Formic acid content is 40～120ppm; Water-content is 80～220ppm, and service temperature reaches 124～128 ℃ at the bottom of the tower, and reflux ratio reaches 3～5; Cause this tower energy consumption higher, and long trioxymethylene of the following residence time of high temperature is prone to decompose again.
Summary of the invention
Method and device that the present invention provides a kind of trioxymethylene to remove light constituent; Increase stripping tower, the increase of stripping tower operation can reduce lightness-removing column column bottom temperature and reflux ratio, cuts down the consumption of energy greatly; Avoid a large amount of decomposition of trioxymethylene, effectively improved trioxymethylene purity.
The technical scheme that the present invention taked is:
A kind of trioxymethylene removes the method for light constituent, comprises the steps:
(1) trioxymethylene, benzene and a spot of water, the organic mixture after will extracting sent into lightness-removing column; 118～122 ℃ of column bottom temperatures; 78～80 ℃ of tower top temperatures; Reflux ratio 1～3 is taken off under pressure 0.1～5Kpa condition gently, and the lightness-removing column overhead gas returns extraction process after the condensation cooling.
(2) mixture that takes off the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace at the bottom of the tower of light back is delivered to stripping tower; Stripping tower with nitrogen as the stripping medium; 115～118 ℃ of column bottom temperatures, 114～117 ℃ of tower top temperatures are carried out stripping under pressure 0.1～5Kpa condition.
Stripping tower adopts stainless steel arc saddle ring filler, and 5～6 of theoretical plate numbers feed the steam coils heat supply in the tower still, and the tower still adopts the chuck attemperator outward, keeps temperature of charge on the one hand, improves gas stripping efficiency on the other hand.
The mass concentration of trioxymethylene is 30%～50% in trioxymethylene after the extraction, benzene and a spot of water, the organic mixture.
At the bottom of the lightness-removing column tower in the mixture of the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace the mass concentration of trioxymethylene greater than 99%.
The device that the present invention also provides a kind of trioxymethylene to remove light constituent comprises lightness-removing column, reboiler, condensate cooler, container for storing liquid, recycle pump, feed-pipe and the 3rd pipeline, also comprises stripping tower and dehvery pump; The opening for feed of stripping tower is connected with the outlet at bottom of lightness-removing column through the pipeline that has dehvery pump; The top of stripping tower and bottom are respectively equipped with first pipeline and second pipeline, and the middle part is provided with nitrogen pipeline.
Adopt the beneficial effect that technique scheme produced to be:
1. increase stripping tower, the increase of stripping operation has reduced the dividing potential drop of light constituent, has broken original vapor liquid equilibrium, makes light component obtain effective elimination, takes off light industry preface product purity and is improved.
2. add the stripping operation, reduced lightness-removing column column bottom temperature and reflux ratio, energy consumption is reduced greatly.
3. the lightness-removing column column bottom temperature reduces, and has effectively avoided a large amount of decomposition of trioxymethylene.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Wherein, 1 lightness-removing column; 2 stripping towers; 3 reboilers; 4 condensate coolers; 5 container for storing liquids; 6 recycle pumps; 7 dehvery pumps; 8 first pipelines; 9 second pipelines; 10 feed-pipes; 11 the 3rd pipelines; 12 nitrogen pipelines.
Embodiment
Embodiment 1
(1) trioxymethylene, benzene and a spot of water, the organic mixture after will extracting sent into lightness-removing column, 120 ℃ of column bottom temperatures; 79 ℃ of tower top temperatures; Reflux ratio 2 is taken off under the pressure 2Kpa condition gently, and the lightness-removing column overhead gas returns extraction process after the condensation cooling.
(2) mixture that takes off the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace at the bottom of the tower of light back is delivered to stripping tower, and as the stripping medium, 117 ℃ of column bottom temperatures, 115 ℃ of tower top temperatures are carried out stripping under the pressure 1Kpa condition to stripping tower with nitrogen.
Through check and analysis, trioxymethylene content is 99.99% at the bottom of the stripping Tata, and methanol content is 27ppm, and formaldehyde content is 28ppm, and formic acid content is 14ppm, and water-content is 22ppm.
Embodiment 2
(1) trioxymethylene, benzene and a spot of water, the organic mixture after will extracting sent into lightness-removing column, 122 ℃ of column bottom temperatures; 79 ℃ of tower top temperatures; Reflux ratio 3 is taken off under the pressure 5Kpa condition gently, and the lightness-removing column overhead gas returns extraction process after the condensation cooling.
(2) mixture that takes off the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace at the bottom of the tower of light back is delivered to stripping tower, and as the stripping medium, 118 ℃ of column bottom temperatures, 116 ℃ of tower top temperatures are carried out stripping under the pressure 5Kpa condition to stripping tower with nitrogen.
Through check and analysis, trioxymethylene content is 99.97% at the bottom of the stripping Tata, and methanol content is 40ppm, and formaldehyde content is 35ppm, and formic acid content is 25ppm, and water-content is 98ppm.
Embodiment 3
(1) trioxymethylene, benzene and a spot of water, the organic mixture after will extracting sent into lightness-removing column, 118 ℃ of column bottom temperatures; 78 ℃ of tower top temperatures; Reflux ratio 1 is taken off under the pressure 0.1Kpa condition gently, and the lightness-removing column overhead gas returns extraction process after the condensation cooling.
(2) mixture that takes off the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace at the bottom of the tower of light back is delivered to stripping tower, and as the stripping medium, 115 ℃ of column bottom temperatures, 114 ℃ of tower top temperatures are carried out stripping under the pressure 0.1Kpa condition to stripping tower with nitrogen.
Through check and analysis, trioxymethylene content is 99.95% at the bottom of the stripping Tata, and methanol content is 115ppm, and formaldehyde content is 128ppm, and formic acid content is 56ppm, and water-content is 80ppm.
Embodiment 4
(1) trioxymethylene, benzene and a spot of water, the organic mixture after will extracting sent into lightness-removing column, 120 ℃ of column bottom temperatures; 80 ℃ of tower top temperatures; Reflux ratio 1.5 is taken off under the pressure 3Kpa condition gently, and the lightness-removing column overhead gas returns extraction process after the condensation cooling.
(2) mixture that takes off the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace at the bottom of the tower of light back is delivered to stripping tower, and as the stripping medium, 115 ℃ of column bottom temperatures, 117 ℃ of tower top temperatures are carried out stripping under the pressure 2Kpa condition to stripping tower with nitrogen.
Through check and analysis, trioxymethylene content is 99.96% at the bottom of the stripping Tata, and methanol content is 57ppm, and formaldehyde content is 60ppm, and formic acid content is 35ppm, and water-content is 87ppm.
Can be found out that by embodiment 1-4 behind the increase stripping process, the purity of the trioxymethylene that obtains improves, the content of formaldehyde, methyl alcohol, formic acid and water obviously reduces.
A kind of trioxymethylene removes the device of light constituent, comprises lightness-removing column 1, reboiler 3, condensate cooler 4, container for storing liquid 5, recycle pump 6, feed-pipe 10 and the 3rd pipeline 11, also comprises stripping tower 2 and dehvery pump 7; The opening for feed of stripping tower 2 is connected with the outlet at bottom of lightness-removing column 1 through the pipeline that has dehvery pump 7; The top of stripping tower 2 and bottom are respectively equipped with first pipeline 8 and second pipeline 9, and the middle part is provided with nitrogen pipeline 12.
During operation; Trioxymethylene after the extraction, benzene and a spot of water, organic mixture; Send into lightness-removing column 1 through feed-pipe 10 and take off gently, lightness-removing column 1 overhead gas is through condensate cooler 4 condensations cooling, again through storage tank 5; A part is returned extraction process through the 3rd pipeline 11, and a part is sent into lightness-removing column 1 and refluxed;
The mixture of the water of trioxymethylene at the bottom of lightness-removing column 1 tower and trace, methyl alcohol, formaldehyde, formic acid etc. is after reboiler 3 heating, and being delivered to stripping tower 2 through dehvery pump 7 carries out stripping, and stripping tower 2 overhead gases get into washing procedure through first pipeline 8 mutually; Liquid is sent into through second pipeline 9 and is taken off the heavy industry preface and take off heavily at the bottom of stripping tower 2 towers.
Nitrogen gets into stripping tower 2 through nitrogen pipeline 12.
Claims (3)
1. a trioxymethylene removes the method for light constituent, it is characterized in that comprising the steps:
(1) trioxymethylene, benzene and a spot of water, the organic mixture after will extracting sent into lightness-removing column; 118～122 ℃ of column bottom temperatures; 78～80 ℃ of tower top temperatures; Reflux ratio 1～3 is taken off under pressure 0.1～5Kpa condition gently, and the lightness-removing column overhead gas returns extraction process after the condensation cooling;
(2) mixture that takes off the water, methyl alcohol, formaldehyde, formic acid etc. of trioxymethylene and trace at the bottom of the tower of light back is delivered to stripping tower; Stripping tower with nitrogen as the stripping medium; 115～118 ℃ of column bottom temperatures, 114～117 ℃ of tower top temperatures are carried out stripping under pressure 0.1～5Kpa condition.
2. a kind of trioxymethylene according to claim 1 removes the method for light constituent, it is characterized in that said stripping tower adopts stainless steel arc saddle ring filler, and 5～6 of theoretical plate numbers feed the steam coils heat supply in the tower still, and the tower still adopts the chuck attemperator outward.
3. a trioxymethylene removes the device of light constituent; Comprise lightness-removing column (1), reboiler (3), condensate cooler (4), container for storing liquid (5), recycle pump (6), feed-pipe (10) and the 3rd pipeline (11), it is characterized in that also comprising stripping tower (2) and dehvery pump (7); The opening for feed of stripping tower (2) is connected with the outlet at bottom of lightness-removing column (1) through the pipeline that has dehvery pump (7); The top of stripping tower (2) and bottom are respectively equipped with first pipeline (8) and second pipeline (9), and the middle part is provided with nitrogen pipeline (12).
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210098979 CN102633770B (en) | 2012-04-06 | 2012-04-06 | Method and device for removing light components in trioxymethylene |
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| CN 201210098979 CN102633770B (en) | 2012-04-06 | 2012-04-06 | Method and device for removing light components in trioxymethylene |
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| CN102633770B CN102633770B (en) | 2013-12-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478848A (en) * | 2015-01-09 | 2015-04-01 | 开封龙宇化工有限公司 | Trioxymethylene light component removal tower separator alkali adding washing device and using method |
| CN108349851A (en) * | 2015-11-06 | 2018-07-31 | 环球油品公司 | C4 absorbers are used to strip the purposes of aldehyde |
| CN110437045A (en) * | 2019-08-26 | 2019-11-12 | 江苏道尔顿石化科技有限公司 | A kind of no alkali cleaning method preparation high-purity metaformaldehyde separating technology |
| CN111514618A (en) * | 2020-04-01 | 2020-08-11 | 南京师范大学 | Purging device, working method and method for removing light polypropylene glycol components |
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| US6201136B1 (en) * | 1998-11-09 | 2001-03-13 | Ticona Gmbh | Separation of liquid mixtures comprising formaldehyde, trioxane, alcohol and hemiformal |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478848A (en) * | 2015-01-09 | 2015-04-01 | 开封龙宇化工有限公司 | Trioxymethylene light component removal tower separator alkali adding washing device and using method |
| CN108349851A (en) * | 2015-11-06 | 2018-07-31 | 环球油品公司 | C4 absorbers are used to strip the purposes of aldehyde |
| CN108349851B (en) * | 2015-11-06 | 2021-05-11 | 环球油品公司 | Use of a C4 absorber for stripping aldehydes |
| CN110437045A (en) * | 2019-08-26 | 2019-11-12 | 江苏道尔顿石化科技有限公司 | A kind of no alkali cleaning method preparation high-purity metaformaldehyde separating technology |
| CN111514618A (en) * | 2020-04-01 | 2020-08-11 | 南京师范大学 | Purging device, working method and method for removing light polypropylene glycol components |
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| CN102633770B (en) | 2013-12-18 |
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