CN100412040C - Chemical grade isoprene recovery method - Google Patents
Chemical grade isoprene recovery method Download PDFInfo
- Publication number
- CN100412040C CN100412040C CNB2006100451764A CN200610045176A CN100412040C CN 100412040 C CN100412040 C CN 100412040C CN B2006100451764 A CNB2006100451764 A CN B2006100451764A CN 200610045176 A CN200610045176 A CN 200610045176A CN 100412040 C CN100412040 C CN 100412040C
- Authority
- CN
- China
- Prior art keywords
- nitric acid
- chemical grade
- dilute nitric
- temperature
- isoprene
- 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.)
- Expired - Fee Related
Links
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000000126 substance Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000011084 recovery Methods 0.000 title claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- XNMQEEKYCVKGBD-UHFFFAOYSA-N dimethylacetylene Natural products CC#CC XNMQEEKYCVKGBD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims abstract description 9
- VWWMOACCGFHMEV-UHFFFAOYSA-N dicarbide(2-) Chemical compound [C-]#[C-] VWWMOACCGFHMEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 2
- 239000010962 carbon steel Substances 0.000 claims description 2
- 210000003298 dental enamel Anatomy 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 229910052573 porcelain Inorganic materials 0.000 claims description 2
- 238000009827 uniform distribution Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004880 explosion Methods 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- 238000005194 fractionation Methods 0.000 abstract 2
- 150000001247 metal acetylides Chemical class 0.000 description 5
- 241000282326 Felis catus Species 0.000 description 4
- 150000001345 alkine derivatives Chemical class 0.000 description 4
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical group CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 150000001993 dienes Chemical class 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000272814 Anser sp. Species 0.000 description 1
- -1 C 5 diene Chemical class 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a method for recovering chemical grade isoptene. The recovery method comprises the procedures of cooling feeding and fractionation, wherein in cooling feeding, materials with the temperature of 50 to 60 DEG C separated through rectification are cooled to 28 to 32 DEG C in secondary extraction analysis, and feeding positions are selected according to the difference of components; in fractionation, operation is carried out under the conditions that operation pressure is from 0.08 to 0.12Mpa at a top, operation pressure is from 0.14 to 0.18Mpa in a kettle, temperature is from 44 to 48 DEG C at the top, temperature is from 62 to 66 DEG C in the kettle, and the reflux ratio is from 8 to 12 chemical grade isoprene is obtained at the bottom of a tower, materials (butyne-2) at the top of the tower enter a dilute nitric acid reactor through a reflux pump, the feeding temperature of butyne-2 is controlled between 34 and 36 DGE C, the concentration of dilute nitric acid is from 8 to 12%, reaction temperature is controlled between 43 and 48 DGE C, and acetylide is completely decomposed. The present invention can obtain chemical grade isoprene by rectification for one time simply without explosion accidents, and safe production is ensured.
Description
(1) technical field under
The present invention relates in carbon five sepn processes recovery once more of being rich in components such as isoprene, alkynes in parsing and the rectifying tower top material, particularly a kind of recovery method of chemical grade isoprene.
(2) background technology
Diolefins such as isoprene, cyclopentadiene, m-pentadiene are rich in a considerable amount of C5 fractions of by-product in the C5 fraction in the petroleum cracking process of producing ethylene.These diolefin chemical property are active, are important chemical material, so it is considerable to carry out carbon five deep processing economic benefits, The goose hangs high has profound significance to the comprehensive utilization petroleum resources.
Cracked C 5 fraction is close by more than 20 kinds of boiling points, the component that easily forms azeotrope is each other formed, therefrom isolate the higher C 5 diene of comprehensive utilization value, (extraction agent is generally DMF to the method for general employing reextraction rectifying, be heated easily to decompose and produce formic acid and diformazan ammonia), its technology is comparatively complicated, for obtaining polymerization grade isoprene, resolve in two collections, rectifying tower top goes out to contain in the material isoprene about 50% and about 30% components such as alkynes, because of alkynes in the ammonia solution of metal-salt, the very sensitive metal acetylide that forms of reaction at a certain temperature explodes strongly and the metal acetylide is heated or clash into easy generation.Therefore when reclaiming two collection parsings, rectifying top isoprene, must remove alkynes or the metal acetylide is decomposed, ensure safety in production.
(3) summary of the invention
The present invention provides a kind of recovery method of chemical grade isoprene in order to remedy the deficiencies in the prior art.This method obtains chemical grade isoprene, and can effectively avoid the metal acetylide to be heated and blast.
The present invention is achieved through the following technical solutions:
A kind of recovery method of chemical grade isoprene, its special character is: comprise the steps:
1) cooling charging: two collections are resolved, to eject temperature be that 50--60 ℃ material is cooled to 28--32 ℃ in rectifying, and 50 layers at the tower middle part of opening for feeds are more than the tower tray, and opening for feed is offered 3-5, looks component different choice feed entrance point;
2) fractionating step: on working pressure top 0.08-0.12Mpa, still 0.14-0.18Mpa, 44--48 ℃ on temperature top, still 62--66 ℃, operate under the condition of reflux ratio 8-12, obtain chemical grade isoprene at the bottom of the tower, directly enter reservoir area chemical grade isoprene finished product jar by tower still discharging pump; Cat head material crotonylene enters the dilute nitric acid reaction device by reflux pump;
3) rare nitric acid, crotonylene enter from dilute nitric acid reaction device bottom, and the crotonylene feed-pipe inserts tower inside, punches on the feed-pipe, make the crotonylene uniform distribution that nebulizes in dilute nitric acid reaction device bottom;
4) reactor operation steps: the crotonylene feeding temperature is controlled at 34--36 ℃; Rare concentration of nitric acid is at 8-12%; Temperature of reaction is controlled at 43-48 ℃; Acetylide decomposes fully;
Chemical grade isoprene product index: the transparent no suspended substance of isoprene 〉=98%.
Further improvement of the present invention is: dilute nitric acid reaction device and dilute nitric acid reaction device eject and set up a gas-liquid equilibrium line between the batch can, and the heat that reaction discharges is effectively controlled, and guarantee to react to carry out smoothly.
Dilute nitric acid reaction equipment matter is carbon steel, and liner enamel (or plastic lining) prevents rare nitric acid corrosion; Dress 25# porcelain ring filler 1.6m in the dilute nitric acid reaction device
3
The present invention proposes a kind of method that adopts rectifying, combines, only need a rectifying, can obtain chemical grade isoprene, and do not have the explosion hazard generation, guarantee safety in production with dilute nitric acid reaction decomposing metal acetylide.
(4) description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Accompanying drawing is the process flow sheet of the recovery method of chemical grade isoprene of the present invention.
Among the figure, 1 isoprene recovery tower, 2 dilute nitric acid reaction devices, 3 dilute nitric acid reaction devices eject batch can, 4 return tanks, 5 interchanger, 6 pumps.
(5) embodiment
Embodiment 1:
Two collections are resolved, rectifying ejects material (50--60 ℃) must be cooled to 30 ℃, enter isoprene recovery tower 1 through fresh feed pump, at working pressure (top 0.1Mpa, still 0.16MPa) temperature (is pushed up 46 ℃, 64.5 ℃ of stills), operate under the condition of reflux ratio 10, obtain chemical grade isoprene at the bottom of the tower, purity is more than 98%, crotonylene, 1-amylene content is all below 0.5%, the cat head isoprene content is below 1.2%, and the cat head material enters dilute nitric acid reaction device 2 through return tank 4 under 35 ℃, and temperature is controlled at about 45 ℃, dilute nitric acid reaction device 2 and dilute nitric acid reaction device eject and set up a gas-liquid equilibrium line between the batch can 3, reaction comparatively relaxes, and acetylide decomposes fully, and rare nitric acid dosage is less.
Embodiment 2:
Two collections are resolved, rectifying ejects material (50--60 ℃) must be cooled to 30 ℃, enter the isoprene recovery tower through fresh feed pump, at working pressure (top 0.12Mpa, still 0.18MPa) temperature (is pushed up 48 ℃, 66 ℃ of stills), operate under the condition of reflux ratio 12, obtain chemical grade isoprene at the bottom of the tower, purity is more than 98%, crotonylene, 1-amylene content is all about 0.8%, the cat head isoprene content enters the dilute nitric acid reaction device below 1% under 35 ℃, temperature is controlled at about 45 ℃, reaction comparatively relaxes, acetylide decomposes fully, rare nitric acid dosage maximum, but energy consumption is bigger.
Embodiment 3:
Two collections are resolved, rectifying ejects material (50--60 ℃) must be cooled to 30 ℃, enter the isoprene recovery tower through fresh feed pump, at working pressure (top 0.08MPa, still 0.14MPa) temperature (is pushed up 44 ℃, 62 ℃ of stills), operate under the condition of reflux ratio 8, obtain chemical grade isoprene at the bottom of the tower, purity is more than 98%, crotonylene, all about 0.5%, the cat head isoprene content enters the dilute nitric acid reaction device to 1-amylene content under 35 ℃ about 2%, temperature is controlled at about 45 ℃, reaction comparatively relaxes, and acetylide decomposes fully, rare nitric acid dosage minimum, the energy consumption minimum, but the isoprene rate of recovery is low.
Claims (4)
1. the recovery method of a chemical grade isoprene is characterized in that: comprise the steps:
1) cooling charging: two collections are resolved, to eject temperature be that 50-60 ℃ material is cooled to 28-32 ℃ in rectifying, and 50 layers at the tower middle part of opening for feeds are more than the tower tray, and opening for feed is offered 3-5, looks component different choice feed entrance point;
2) fractionating step: on working pressure top 0.08-0.12Mpa, still 0.14-0.18Mpa, 44-48 ℃ on temperature top, still 62--66 ℃, operate under the condition of reflux ratio 8-12, obtain chemical grade isoprene at the bottom of the tower, directly enter reservoir area chemical grade isoprene finished product jar by tower still discharging pump; Cat head material crotonylene enters the dilute nitric acid reaction device by reflux pump;
3) rare nitric acid, crotonylene enter from dilute nitric acid reaction device bottom, and the crotonylene feed-pipe inserts tower inside, punches on the feed-pipe, make the crotonylene uniform distribution that nebulizes in dilute nitric acid reaction device bottom;
4) reactor operation steps: the crotonylene feeding temperature is controlled at 34--36 ℃; Rare concentration of nitric acid is at 8-12%; Temperature of reaction is controlled at 43-48 ℃; Acetylide decomposes fully; Chemical grade isoprene product index: the transparent no suspended substance of isoprene 〉=98%.
2. the recovery method of chemical grade isoprene according to claim 1, it is characterized in that: dilute nitric acid reaction device and dilute nitric acid reaction device eject and set up a gas-liquid equilibrium line between the batch can.
3. the recovery method of chemical grade isoprene according to claim 1, it is characterized in that: dilute nitric acid reaction equipment matter is carbon steel, liner prevents rare nitric acid corrosive enamel or plastic lining.
4. the recovery method of chemical grade isoprene according to claim 1 is characterized in that: dress 25# porcelain ring filler 1.6m in the dilute nitric acid reaction device
3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100451764A CN100412040C (en) | 2006-06-29 | 2006-06-29 | Chemical grade isoprene recovery method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100451764A CN100412040C (en) | 2006-06-29 | 2006-06-29 | Chemical grade isoprene recovery method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1876607A CN1876607A (en) | 2006-12-13 |
| CN100412040C true CN100412040C (en) | 2008-08-20 |
Family
ID=37509197
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2006100451764A Expired - Fee Related CN100412040C (en) | 2006-06-29 | 2006-06-29 | Chemical grade isoprene recovery method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100412040C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503758A (en) * | 2011-11-02 | 2012-06-20 | 天津渤海化工有限责任公司天津碱厂 | Method for reducing benzene consumption in production process of polyformaldehyde |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412165A (en) * | 2001-10-12 | 2003-04-23 | 中国石油化工股份有限公司 | Separation method of cracked C5 fraction |
-
2006
- 2006-06-29 CN CNB2006100451764A patent/CN100412040C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1412165A (en) * | 2001-10-12 | 2003-04-23 | 中国石油化工股份有限公司 | Separation method of cracked C5 fraction |
Non-Patent Citations (2)
| Title |
|---|
| 碳四碳五烯烃工学. 张旭之等，593－598，600－601，化学工业出版社. 1998 |
| 碳四碳五烯烃工学. 张旭之等，593－598，600－601，化学工业出版社. 1998 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1876607A (en) | 2006-12-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1162380C (en) | Separation method of cracked C5 fraction | |
| CN101143805B (en) | Method for separating phenols compounds from phenol-containing raw material oil | |
| CN105566032B (en) | The selection hydrogenation technique of rich alkynes carbon four | |
| CN104726134B (en) | Method for producing high-quality gasoline/diesel from chlorine-containing plastic oil | |
| CN100551925C (en) | The synthetic process of triethyl aluminum | |
| CN100412040C (en) | Chemical grade isoprene recovery method | |
| CN104829408A (en) | Method for separating ethyl acetate and cyclohexane | |
| CN101838177A (en) | Method for one-stage extraction, distillation and separation of C5 fractions by using reactive distillation N-methyl pyrrolidone (NMP) method | |
| CN102311771A (en) | Crude oil processing method | |
| CN111440057A (en) | Preparation method for producing anhydrous formaldehyde by extractive distillation | |
| CN103183579B (en) | Separation system and separation method for piperylene and dicyclopentadiene | |
| CN208762430U (en) | The anti-corrosive apparatus of methyl acetate hydrolysis and acetic acid refining during polyvinyl alcohol disposing mother liquor | |
| CN109663387B (en) | Degassing and deodorizing method for carbon black water of acetylene device | |
| CN106701182B (en) | The method of cracking carbon nine cut fraction hydrogenation | |
| CN217247965U (en) | Tail gas recovery device for propionyl chloride production | |
| CN109181751A (en) | A kind of light aromatic hydrocarbons add hydrogen transformation device and operating method | |
| CN104030872B (en) | A kind of method improving acetonitrile method 1,3-butadiene extraction plant raffinate product yield | |
| CN101386572A (en) | Method for separating and purifying acetylacetone | |
| CN106478455A (en) | The removal methods of micro hydrocyanic acid in acetonitrile refining system | |
| CN104560148A (en) | Light gasoline catalytic rectification etherification device and technique | |
| CN102329186A (en) | Method for preparing high-purity 1,2-butadiene by batch rectification method of ice water condensation | |
| CN104230972A (en) | Method for purifying anisole-boron trifluoride complex | |
| CN221192081U (en) | System for degree of depth improves vacuum tower side line product quality | |
| CN204111631U (en) | A kind of trialkyl indium-etherate takes off ether device | |
| CN212189034U (en) | Curing agent recycling and processing system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Chemical grade isoprene recovery method Effective date of registration: 20120719 Granted publication date: 20080820 Pledgee: Prudential Bank Ji'nan branch of Limited by Share Ltd. Pledgor: SHANDONG YUHUANG CHEMICAL Co.,Ltd. Registration number: 2012990000388 |
|
| ASS | Succession or assignment of patent right |
Owner name: SHANDONG YUHUANG SHENGSHI CHEMICAL CO., LTD. Free format text: FORMER OWNER: SHANDONG YUHUANG CHEMICAL CO., LTD. Effective date: 20141126 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 274500 HEZE, SHANDONG PROVINCE TO: 274000 HEZE, SHANDONG PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20141126 Address after: 274000 Changjiang Road, Heze Development Zone, Shandong, China, No. 4666 Patentee after: Jade Emperor flourishing age chemical Inc. Shandong Address before: 274500 Shandong city of Heze province Dongming County wusheng Township Development Zone Patentee before: SHANDONG YUHUANG CHEMICAL Co.,Ltd. |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PM01 | Change of the registration of the contract for pledge of patent right |
Change date: 20150713 Registration number: 2012990000388 Pledgor after: Jade Emperor flourishing age chemical Inc. Shandong Pledgor before: SHANDONG YUHUANG CHEMICAL Co.,Ltd. |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20150721 Granted publication date: 20080820 Pledgee: Prudential Bank Ji'nan branch of Limited by Share Ltd. Pledgor: Jade Emperor flourishing age chemical Inc. Shandong Registration number: 2012990000388 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Chemical grade isoprene recovery method Effective date of registration: 20150910 Granted publication date: 20080820 Pledgee: China Minsheng Banking Corp Ji'nan branch Pledgor: Jade Emperor flourishing age chemical Inc. Shandong Registration number: 2015370000047 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20180704 Granted publication date: 20080820 Pledgee: China Minsheng Banking Corp Ji'nan branch Pledgor: Jade Emperor flourishing age chemical Inc. Shandong Registration number: 2015370000047 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20080820 |