CN104628538A - Synthetic method of dibutyl ether - Google Patents
Synthetic method of dibutyl ether Download PDFInfo
- Publication number
- CN104628538A CN104628538A CN201310546280.1A CN201310546280A CN104628538A CN 104628538 A CN104628538 A CN 104628538A CN 201310546280 A CN201310546280 A CN 201310546280A CN 104628538 A CN104628538 A CN 104628538A
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- CN
- China
- Prior art keywords
- dibutyl ether
- synthetic method
- heated
- crude product
- subjected
- 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.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/09—Preparation of ethers by dehydration of compounds containing hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a synthetic method of dibutyl ether. The synthetic method comprises following steps: n-butyl alcohol and concentrated sulfuric acid are delivered into a reactor provided with a reflux unit at a certain ratio; an obtained mixture is heated to 120 to 140 DEG C in the presence of a catalyst, and is subjected to full reaction for 1.5h; a reaction residue is cooled, water with a same volume is added, oil phase is removed, water phase is heated for evaporation dewatering, temperature is increased to 200 DEG C further, and steam is collected and is subjected to condensation so as to obtain a dibutyl ether crude product; and the dibutyl ether crude product is washed with saturated sodium chloride solution for 2 to 4 times so as to obtain a dibutyl ether refined product. The process of the synthetic method is easy to control; purity of the obtained dibutyl ether refined product is high; the production technology is compact; and byproducts are few.
Description
Technical field
The present invention relates to a kind of industrial chemicals synthetic method, be specifically related to a kind of synthetic method of dibutyl ether.
Background technology
Dibutyl ether has very strong solvency power to many natural and Synthetic Oil, resin, rubber, organic acid acetic, alkaloid etc., toxicity and danger little, be the very high solvent of security, the mixing solutions of the extraction and refining solvent and butyl phosphate that are widely used as resin, grease, organic acid, ester, wax, alkaloid, hormone etc. can be used as the solvent of separation of rare earth elements.Simultaneously because butyl ether is inert solvent, also can be used as the organic synthesis solvent of Grignard reagent, rubber, agricultural chemicals etc.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, provides a kind of synthetic method of new dibutyl ether.
Technical problem to be solved by this invention is realized by following technical scheme.The present invention is a kind of synthetic method of dibutyl ether, be characterized in: propyl carbinol and the vitriol oil are put in the reactor with reflux according to certain formula rate, under the effect of catalyzer, be heated to 120-140 DEG C, abundant reaction 1.5 hours, reaction residual is cooled, add isopyknic water, remove oil phase, by heated aqueous dehydration by evaporation, temperature is brought up to 200 DEG C further, vapor collection condensation is dibutyl ether crude product, then dibutyl ether saturated sodium chloride solution washing is dibutyl ether fine work for 2-4 time.
Compared with prior art, process of the present invention is easy to control, and product dibutyl ether purity is high, and meanwhile, whole production technique is compact, and byproduct is few.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art understands the present invention further, and do not form the restriction to its right.
Embodiment 1, a kind of synthetic method of dibutyl ether, propyl carbinol and the vitriol oil are put in the reactor with reflux according to the formula rate of volume ratio 2: 1, under the effect of catalyzer, be heated to 140 DEG C, abundant reaction 1.5 hours, reaction residual is cooled, add isopyknic water, remove oil phase, by heated aqueous to 100 DEG C dehydration by evaporation, temperature is brought up to 200 DEG C further, vapor collection condensation is dibutyl ether crude product, then dibutyl ether is washed 4 times with saturated sodium chloride solution and be dibutyl ether fine work.
Claims (4)
1. a synthetic method for dibutyl ether, is characterized in that raw materials used for propyl carbinol and the vitriol oil, according to certain formula rate through adding thermal synthesis, dealcoholysis, dehydration, distillation, washing form.
2. the synthetic method of a kind of dibutyl ether according to claim 1, is characterized in that described formula is that propyl carbinol and the vitriol oil are according to volume ratio 2: 1.
3. the synthetic method of a kind of dibutyl ether according to claim 1, is characterized in that described synthesis is reactor propyl carbinol and the vitriol oil put into reflux, under the effect of catalyzer, is heated to 140 DEG C, fully reaction 1.5 hours.
4. the synthetic method of a kind of dibutyl ether according to claim 1, is characterized in that described washing is with saturated sodium chloride solution washing 2-4 time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310546280.1A CN104628538A (en) | 2013-11-07 | 2013-11-07 | Synthetic method of dibutyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310546280.1A CN104628538A (en) | 2013-11-07 | 2013-11-07 | Synthetic method of dibutyl ether |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104628538A true CN104628538A (en) | 2015-05-20 |
Family
ID=53207835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310546280.1A Pending CN104628538A (en) | 2013-11-07 | 2013-11-07 | Synthetic method of dibutyl ether |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104628538A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111534033A (en) * | 2020-06-15 | 2020-08-14 | 扬州爱非科鞋业有限公司 | Preparation method of anti-slip sole |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101472871A (en) * | 2006-06-16 | 2009-07-01 | 纳幕尔杜邦公司 | Process for making dibutyl ethers from aqueous 1-butanol |
| CN101541720A (en) * | 2006-12-01 | 2009-09-23 | 纳幕尔杜邦公司 | Process for making dibutyl ethers from dry ethanol |
| CN101796010A (en) * | 2007-09-05 | 2010-08-04 | 纳幕尔杜邦公司 | Processes for making dialkyl ethers from alcohols |
-
2013
- 2013-11-07 CN CN201310546280.1A patent/CN104628538A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101472871A (en) * | 2006-06-16 | 2009-07-01 | 纳幕尔杜邦公司 | Process for making dibutyl ethers from aqueous 1-butanol |
| CN101541720A (en) * | 2006-12-01 | 2009-09-23 | 纳幕尔杜邦公司 | Process for making dibutyl ethers from dry ethanol |
| CN101796010A (en) * | 2007-09-05 | 2010-08-04 | 纳幕尔杜邦公司 | Processes for making dialkyl ethers from alcohols |
Non-Patent Citations (2)
| Title |
|---|
| 王俊茹: "高产率制备正丁醚", 《天津化工》, no. 3, 31 December 1998 (1998-12-31), pages 38 - 39 * |
| 范平等: "微波常压法合成正丁醚", 《辽宁大学学报 自然科学版》, vol. 29, no. 1, 31 December 2002 (2002-12-31), pages 62 - 63 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111534033A (en) * | 2020-06-15 | 2020-08-14 | 扬州爱非科鞋业有限公司 | Preparation method of anti-slip sole |
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| Date | Code | Title | Description |
|---|---|---|---|
| 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 |
Application publication date: 20150520 |