CN1125711A - Method for seperating high boiling point composition from coarse butynediol - Google Patents
Method for seperating high boiling point composition from coarse butynediol Download PDFInfo
- Publication number
- CN1125711A CN1125711A CN95115579A CN95115579A CN1125711A CN 1125711 A CN1125711 A CN 1125711A CN 95115579 A CN95115579 A CN 95115579A CN 95115579 A CN95115579 A CN 95115579A CN 1125711 A CN1125711 A CN 1125711A
- Authority
- CN
- China
- Prior art keywords
- high boiling
- cymogene
- butynediol
- tower
- boiling point
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C33/00—Unsaturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C33/04—Acyclic alcohols with carbon-to-carbon triple bonds
- C07C33/042—Acyclic alcohols with carbon-to-carbon triple bonds with only one triple bond
- C07C33/044—Alkynediols
- C07C33/046—Butynediols
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method for separating high boiling point distillate from crude butynediol solution which is purified from other unexpected components is provided. The unexpected components refer to acetylene, formaldehyde, propargyl alcohol, etc. wherein, the high boiling point distillate is separated from the crude butynediol solution in a flashing column. The temperature of the crude butynediol solution supplied to the flashing column is between 120 DEG C and 170 DEG C and the pressure between 5 millibar and 50 millibar.
Description
The present invention relates to a kind of method of separating heavy cut from other undesirable component from the cymogene alkyne diol solution of having purified, described undesirable component resembles for example acetylene, formaldehyde, propargyl alcohol etc.
The acetylene, nonreactive formaldehyde, propargyl alcohol and other lower boiling and the high boiling component that also contain physical dissolution by the synthetic cymogene alkyne diol solution that obtains of butynediol.As everyone knows, isolate acetylene and then cymogene alkyne diol solution is sent into two vacuum towers that are provided with continuously by stripping tower.In first vacuum tower, from cymogene alkyne diol solution, remove formaldehyde and low boiling component, and in second vacuum tower, separate high boiling component, and obtain pure butyne diol solutions through the top (referring to for example, Chem System Inc., Butanediol/Tetrahydrofuran-Report, Nr.91S15, in April, 1993, the 22 page, Fig. 2, B.1).In the case, be the distillation 5 to 20 millibar under carried out in second vacuum tower less than 145 ℃ with pressure at Wen Gaowei.These parameters are very important, so that reach goodish distillation, that is, generate other polymkeric substance by butynediol and keep low as far as possible.In used currently known methods, the vacuum distilling separating formaldehyde will cause the cymogene alkyne diol solution of the removing formaldehyde in the first vacuum tower groove moisture hardly.Increased the generation of high boiling component in first distillation by boiling of cymogene alkyne diol solution.The composition of sending out owing to the high boiling point group that plays interference effect in hydrogenation is too high, as described above, and must isolate these components in another vacuum tower.The high boiling component that generates in catalysis synthesizing butynediol and the method steps followed must separate before the butynediol catalytic hydrogenation, because they will cause damaging product and infringement hydrogenation catalyst.Because cymogene alkyne diol solution residence time in second vacuum tower is long, therefore wherein also can produces other polymkeric substance or generate high boiling component.In addition, the tower that need use of vacuum distilling is very expensive and difficult with operation.
The objective of the invention is from cymogene alkyne diol solution, to isolate heavy cut with simple method.
According to the present invention, so reach this purpose, promptly in a flashing tower, from cymogene alkyne diol solution, isolate heavy cut.Now replace up to the present used vacuum tower with a flash distillation.With in vacuum column, compare the residence time much shorter of fraction in tower that enters the cymogene alkyne diol in the flashing tower or in flashing tower top and groove, obtain.Therefore can reduce the generation of polymkeric substance or high boiling component substantially.Owing to have enough big boiling temperature poor between butynediol and high boiling component, therefore, can in flashing tower, from the butynediol that obtains at cat head, isolate high boiling component, its amount is in step of hydrogenation after this in the limit of regulation.
Form the inventive method and be characterised in that, supply with temperature that the cymogene alkyne diol solution of flashing tower had between 120 and 170 ℃, pressure is between 5 and 50 millibars.
Produced laboratory test, under 140 ℃ of temperature and 5 millibars of pressure, can produce the butynediol fraction with 99.5 (quality) % in the groove of this tower in flashing tower, it only also contains 0.1 (quality) % high boiling component.
Generally speaking, compare with currently known methods to conclude, method of the present invention has lot of advantages.Therefore, can abandon one and compare much expensive vacuum tower with flashing tower.In addition, compare with vacuum tower, flashing tower is more easy to control.Because flashing tower does not have internal structure, resembling does not for example have column plate or filler, so its important running cost is much lower.In common distillation tower, along with time lapse, the internal structure just by high boiling component is clung promptly can produce the no small pressure-losses in some cases.Reason importantly will clean column plate constantly thus.These cleanings can be cancelled when separating high boiling component with flashing tower.
Claims (2)
- The method of 1, from the cymogene alkyne diol solution of from other undesirable component, having purified, separating heavy cut, described undesirable component resembles for example acetylene, formaldehyde, propargyl alcohol etc., it is characterized in that, in a flashing tower, from cymogene alkyne diol solution, isolate heavy cut.
- 2, according to the method for claim 1, it is characterized in that, supply with temperature that the cymogene alkyne diol solution of flashing tower had between 120 and 170 ℃, pressure is between 5 and 50 millibars.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4432581A DE4432581C2 (en) | 1994-09-13 | 1994-09-13 | Process for separating the high boiler fraction from a crude butynediol solution |
| DEP4432581.9 | 1994-09-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1125711A true CN1125711A (en) | 1996-07-03 |
Family
ID=6528102
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95115579A Pending CN1125711A (en) | 1994-09-13 | 1995-08-28 | Method for seperating high boiling point composition from coarse butynediol |
Country Status (4)
| Country | Link |
|---|---|
| KR (1) | KR100369972B1 (en) |
| CN (1) | CN1125711A (en) |
| DE (1) | DE4432581C2 (en) |
| TW (1) | TW297020B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101253138B (en) * | 2005-09-06 | 2011-06-15 | 巴斯夫欧洲公司 | Method for the separation of polymeric by-products from 1,4-butynediol |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005042184A1 (en) * | 2005-09-06 | 2007-03-08 | Basf Ag | Process for the separation of polymeric by-products from 1,4-butynediol |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1063147B (en) * | 1956-08-07 | 1959-08-13 | Basf Ag | Process for the preparation of butyne-2-diol-1, 4 |
-
1994
- 1994-09-13 DE DE4432581A patent/DE4432581C2/en not_active Expired - Fee Related
-
1995
- 1995-08-26 KR KR1019950026779A patent/KR100369972B1/en not_active IP Right Cessation
- 1995-08-28 CN CN95115579A patent/CN1125711A/en active Pending
- 1995-09-30 TW TW084110225A patent/TW297020B/zh active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101253138B (en) * | 2005-09-06 | 2011-06-15 | 巴斯夫欧洲公司 | Method for the separation of polymeric by-products from 1,4-butynediol |
Also Published As
| Publication number | Publication date |
|---|---|
| TW297020B (en) | 1997-02-01 |
| DE4432581C2 (en) | 1997-01-23 |
| DE4432581A1 (en) | 1996-03-14 |
| KR960010599A (en) | 1996-04-20 |
| KR100369972B1 (en) | 2003-05-23 |
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Legal Events
| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| REG | Reference to a national code |
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