CN1370774A - Butylene oxide recovering process - Google Patents
Butylene oxide recovering process Download PDFInfo
- Publication number
- CN1370774A CN1370774A CN 01103145 CN01103145A CN1370774A CN 1370774 A CN1370774 A CN 1370774A CN 01103145 CN01103145 CN 01103145 CN 01103145 A CN01103145 A CN 01103145A CN 1370774 A CN1370774 A CN 1370774A
- Authority
- CN
- China
- Prior art keywords
- thf
- tetrahydrofuran
- waste liquid
- sodium hydroxide
- ethanol
- 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
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004821 distillation Methods 0.000 claims abstract description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 88
- 239000007788 liquid Substances 0.000 claims description 25
- 239000002699 waste material Substances 0.000 claims description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 7
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- QCDFBFJGMNKBDO-UHFFFAOYSA-N Clioquinol Chemical compound C1=CN=C2C(O)=C(I)C=C(Cl)C2=C1 QCDFBFJGMNKBDO-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 abstract 2
- 239000006227 byproduct Substances 0.000 abstract 1
- 125000004494 ethyl ester group Chemical group 0.000 abstract 1
- 229940088597 hormone Drugs 0.000 abstract 1
- 239000005556 hormone Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000543 intermediate Substances 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 229960004249 sodium acetate Drugs 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a recovering process of butylene oxide, which exists in one multiple-component mixture as side product in cortial hormone production. Mixed dissolvent with butylenes oxide as main components is first obtained through distillation process, its ethyl ester is hydrolyzed with sodium hydroxide and its ethanol content is reduced to below 0.2 % through water washing process, and through sodium hydroxide dewatering and rectification butylenes oxide product is produced. The present invention has simple process, high yield and high safety and reliability.
Description
The invention belongs to from containing 10%---reclaim the technology of tetrahydrofuran (THF) the skin waste liquid of 20% tetrahydrofuran (THF).
That produces the cortin generation now contains 10%---and 20% tetrahydrofuran (THF) waste liquid no longer therefrom reclaims tetrahydrofuran (THF) as offal treatment.
The objective of the invention is to seek a kind of yield height, pollute and lack, the safe and reliable technology that is suitable for industrial recovery tetrahydrofuran (THF) by the cortin that contains tetrahydrofuran (THF) is produced waste liquid recycling.
The tetrahydrofuran (THF) waste liquid is a three-phase liquid, and water, tetrahydrofuran (THF), ethyl acetate are multicomponent mixtures, utilizes distillating method to obtain the solvent that tetrahydrofuran (THF) accounts for major ingredient, and water and inorganics are removed.Utilize sodium hydroxide hydrolysis second fat to become sodium-acetate and ethanol to introduce toluene again and wash for extraction agent, utilize the dissolubility difference of tetrahydrofuran (THF) and ethanol and toluene and water, the method for washing with water is removed ethanol.Remove the alcoholic acid tetrahydrofuran (THF) and obtain the tetrahydrofuran (THF) finished product through the essence steaming with the sodium hydroxide dehydration.The tetrahydrofuran (THF) that washing ethanol is taken away utilizes ethanol and tetrahydrofuran (THF) boiling point difference to distill to such an extent that tetrahydrofuran (THF) is applied mechanically down in batch extraction again.
The present invention is achieved in that and will contains 10%---the cortin waste liquid of 20% tetrahydrofuran (THF) is squeezed into the branch flow container and was left standstill 24 hours, then the second fat on upper strata is removed; The remaining tetrahydrofuran (THF) waste liquid that contains is squeezed into extractor and distilled, and retort gas reaches 55---and 90 degree obtain intermediate; In this intermediate, adding 20%---30% sodium hydroxide is hydrolyzed to second fat wherein, discards alkali lye; Add 45% again---the water of 55% toluene and 0.4 cubic metre/ton, stir the back standing demix, remove ethanol wherein, make ethanol content less than 0.2%, hydrolyzed solution distills once more removes part ethanol and following batch of extraction applied mechanically;---1.5% sodium hydroxide dehydration discards alkali lye: extraction liquid is squeezed into the smart jar that steams carry out essence and steam, smart steam body reaches 65---70 that add 0.5% again obtains tetrahydrofuran (THF) when spending, and the low tetrahydrofuran (THF) that boils is applied mechanically with following batch of extraction.
Technology of the present invention is simple, and is safe and reliable, and yield is up to 8.9%, and the tetrahydrofuran (THF) of recovery reaches industry standard.Excellent beneficial effect of the present invention is confirmed by following experimental result:
| Numbering | Material name | Waste liquid amount | Content | Method | Finished product | Yield | Quality standard |
| ????1 | The tetrahydrofuran (THF) waste liquid | 1000g | ?14 ?％ | Existing method | 90g | ?9.0％ | In-house standard |
| ????2 | The tetrahydrofuran (THF) waste liquid | 1000g | ?15 ?％ | Existing method | 89g | ?8.9％ | In-house standard |
| ????3 | The tetrahydrofuran (THF) waste liquid | 1000g | ?16 ?％ | Existing method | 89g | ?8.9％ | In-house standard |
| ????4 | The tetrahydrofuran (THF) waste liquid | 1000g | ?15 ?％ | Existing method | 90g | ?9.0％ | In-house standard |
| ????5 | The tetrahydrofuran (THF) waste liquid | 1000g | ?14 ?％ | Existing method | 91g | ?9.1％ | In-house standard |
| ????6 | The tetrahydrofuran (THF) waste liquid | 1000g | ?13 ?％ | Existing method | 88g | ?8.8％ | In-house standard |
| ????7 | The tetrahydrofuran (THF) waste liquid | 1000g | ?14 ?％ | Existing method | 89g | ?8.9％ | In-house standard |
| ????8 | The tetrahydrofuran (THF) waste liquid | 1000g | ?15 ?％ | Existing method | 89g | ?8.9％ | In-house standard |
| ????9 | The tetrahydrofuran (THF) waste liquid | 1000g | ?15 ?％ | Existing method | 89g | ?8.9％ | In-house standard |
Embodiment 1
Three distillations of 21 tons of branches of tetrahydrofuran (THF) waste liquid (telling ethanol 300L before the distillation), distillation obtains 6 tons of intermediates (every batch approximately goes out 2 tons of intermediates) and adds 500kg sheet basic hydrolysis second fat and tell alkali lye 400L and put into trench, add 3.5 tons of toluene again, 1 ton of water, stirred 40 minutes, left standstill 40 minutes, divide water to be divided into out 1.4 tons of water and put into trench, adding 1 ton of water again stirred 40 minutes, left standstill 40 minutes, divide water to go into the ground jar, repeat this operation totally 10 times, add the dehydration of 75kg sodium hydroxide again below 0.2% with ethanol content in the gas chromatograph survey tetrahydrofuran (THF), stirred 30 minutes, left standstill 10 minutes, and divided buck 100L to go into trench, extraction liquid is squeezed into the smart jar that steams, and steams through essence to obtain 1.2 tons of tetrahydrofuran (THF) finished products.
Totally 14 tons in ground jar water slightly steams, extracts smart the steaming at twice and obtains 0.7 ton of tetrahydrofuran (THF) finished product.
Embodiment 2
Three distillations of 21 tons of branches of tetrahydrofuran (THF) waste liquid (telling second fat 300L before the distillation) distillation obtains 6.2 tons of intermediates (every batch approximately goes out 2 tons of intermediates), add 500kg sheet alkali, in the hydrolysis tetrahydrofuran (THF) second fat make it to become ethanol and sodium-acetate alkali lye altogether 420L put into trench, add 3.5 tons of toluene again, 1 ton of water stirred 40 minutes, left standstill 40 minutes, divide water to go into the ground jar, repeat aforesaid operations 10 times, be washed till that ethanol content is below 0.2% in the tetrahydrofuran (THF), hydro-oxidation sodium 75kg dewaters, stirred 30 minutes, left standstill 10 minutes, and divided alkali lye to go into trench, again extraction liquid is obtained 1.4 tons of tetrahydrofuran (THF) finished products through the essence steaming.
Totally 14 tons in ground jar water slightly steams at twice, extraction again, and smart the steaming obtains 0.8 ton of tetrahydrofuran (THF) finished product.
Claims (3)
1. one kind from containing 10%---reclaim the technology of tetrahydrofuran (THF) the cortin waste liquid of 20% tetrahydrofuran (THF), after it is characterized in that this waste liquid left standstill, divide and remove part second fat, then, the remaining tetrahydrofuran (THF) waste liquid that contains is distilled, retort gas reaches 55---90 degree, obtain intermediate, in this intermediate, adding 20%---30% sodium hydroxide is hydrolyzed to second fat wherein, discard alkali lye, adding 45% again---55% toluene is made extraction agent and is washed method with water and remove wherein ethanol, and---carry out essence steaming after the dehydration of 1.5% sodium hydroxide, smart steam body reaches 65---70 that add 0.5% again obtains tetrahydrofuran (THF) when spending.
2. method according to claim 1 is characterized in that extracting the hydrolyzed solution that obtains, and distillation is removed part ethanol and following batch of extraction and applied mechanically once more.
3. method according to claim 1 is characterized in that smart steam boil tetrahydrofuran (THF) and following batch of extraction of obtain low and applying mechanically.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01103145 CN1370774A (en) | 2001-02-27 | 2001-02-27 | Butylene oxide recovering process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01103145 CN1370774A (en) | 2001-02-27 | 2001-02-27 | Butylene oxide recovering process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1370774A true CN1370774A (en) | 2002-09-25 |
Family
ID=4653139
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01103145 Pending CN1370774A (en) | 2001-02-27 | 2001-02-27 | Butylene oxide recovering process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1370774A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555238B (en) * | 2009-05-21 | 2011-02-09 | 广西万德药业股份有限公司 | Method for tetrahydrofuran recycling |
| CN102557859A (en) * | 2012-01-04 | 2012-07-11 | 扬州市丽邦化工有限公司 | Method for separating mixed solvent of tetrahydrofuran, acetic ether and methylbenzene |
| WO2018039848A1 (en) * | 2016-08-29 | 2018-03-08 | 沈建美 | Recovery process for tetrahydrofuran |
-
2001
- 2001-02-27 CN CN 01103145 patent/CN1370774A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555238B (en) * | 2009-05-21 | 2011-02-09 | 广西万德药业股份有限公司 | Method for tetrahydrofuran recycling |
| CN102557859A (en) * | 2012-01-04 | 2012-07-11 | 扬州市丽邦化工有限公司 | Method for separating mixed solvent of tetrahydrofuran, acetic ether and methylbenzene |
| WO2018039848A1 (en) * | 2016-08-29 | 2018-03-08 | 沈建美 | Recovery process for tetrahydrofuran |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |