CN105001057A - Preparation method of 2-methylbutanol - Google Patents
Preparation method of 2-methylbutanol Download PDFInfo
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- CN105001057A CN105001057A CN201510484045.5A CN201510484045A CN105001057A CN 105001057 A CN105001057 A CN 105001057A CN 201510484045 A CN201510484045 A CN 201510484045A CN 105001057 A CN105001057 A CN 105001057A
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- preparation
- methyl butanol
- reaction
- 1mpa
- butanol according
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- 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
- C07C29/17—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds
- C07C29/175—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrogenation of carbon-to-carbon double or triple bonds with simultaneous reduction of an oxo group
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- 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
Abstract
The invention discloses a preparation method of 2-methylbutanol, and belongs to the field of fine chemical engineering. 2-ethyl acrolein is adopted as raw materials, a crude product of the 2-methylbutanol is obtained through catalytic reduction, then the catalytic reduction is separated out through rectification, and the GC content is larger than or equal to 99.5 percent.
Description
Technical field
The invention belongs to field of fine chemical, be specifically related to a kind of preparation method of organic raw material 2-methyl butanol.
Background technology
2-methyl butanol is widely used in the production of various food-drink, tobacco and wine, daily necessities, and at home and abroad market is very popular.Chinese invention applies for a patent in CN200310106387.0 and CNCN97104420.1 the preparation method disclosing preparation 2-methyl butanol, mainly with grain or other natural phant for raw material, the by product fusel that fermentation produces carries out rectifying separation and obtains 2-methyl butanol.The GC content of the 2-methyl butanol extracted in above-mentioned preparation method is only about 98%.
In order to meet the growing market requirement better, provide more highly purified product, developing the method for chemosynthesis, to obtain 2-methyl butanol extremely urgent.
Summary of the invention
The present invention, in order to overcome above-mentioned defect, provides a kind of chemical preparation process of 2-methyl butanol.By technique provided by the invention, amplify after producing, GC content >=99.5% of the 2-methyl butanol obtained.
A preparation method for 2-methyl butanol, is characterized in that comprising the steps and processing condition:
(1) in autoclave, drop into 2-ethyl acrylic aldehyde, catalysts and solvents, adopt nitrogen replacement reaction system, then blow three times with hydrogen, then close relief valve, be filled with hydrogen in still, pressure-controlling is at 0.1-1MPa.
(2) reaction at temperature control 0-80 DEG C, still internal pressure carries out reduction reaction at 0.1-1MPa, insulation reaction 3-5 hour.
(3) after above-mentioned (2) have reacted, filtering recovering catalyst, reusable edible 5-8 time.
(4) filtrate of above-mentioned (3) is transferred to rectifying tower, obtains product after rectifying, yield 85-98%, GC >=99.5%.
Further, in technique scheme, described catalyzer is platinum carbon or Raney's nickel.
Further, in technique scheme, described solvent is methyl alcohol, ethanol, Virahol, ethyl acetate or tetrahydrofuran (THF).
Further, in technique scheme, described 2-ethyl acrylic aldehyde, catalyst weight are than being 1:0.01-0.1.
Further, in technique scheme, described reduction reaction temperature 0-80 DEG C.
Further, in technique scheme, described reacting kettle inner pressure is at 0.1-1MPa.
the beneficial effect of the invention:
(1) in synthetic technology: adopt 2-ethyl acrylic aldehyde to make raw material, synthesis yield is high, favorable reproducibility, process stabilizing.
(2) in economic benefit: not only provide more choices for domestic and international chemical enterprise after this product industrialization, and will purchase convenient, economical.Raw material sources are extensive, cheap and easy to get, and catalyzer repeatedly can recycled, and economic benefit is obvious.
(3) at quality product aspect of performance: because product purity is up to more than 99.5%, client can directly use, and without the need to purifying, improves production efficiency again.
Embodiment
embodiment 1:
20 kilograms of 2-ethyl acrylic aldehyde, 200 gram of 5% platinum carbon, 50 kg ethanol are added successively in the autoclave of 100L, with nitrogen replacement reactive system three times, then blow three times with hydrogen, then close relief valve, open hydrogen gas valve, until autoclave internal pressure reaches 0.1MPa.Close intake valve, be then heated to 30 DEG C ± 2 DEG C, and insulation reaction 3 hours at this temperature, supplement logical hydrogen twice in the middle of this process needs, till reaction no longer absorbs hydrogen.Cooling, release, by reacting liquid filtering, reclaims catalyzer (being directly used in the reaction of embodiment 2), then by upper for filtrate tower rectifying, isolates desired product 2-methyl butanol 19.5 kilograms, GC content 99.7%, yield 93.1%.
embodiment 2:
Add successively in the autoclave of 100L in 20 kilograms of 2-ethyl acrylic aldehyde, above-described embodiment 1 and reclaim catalyzer, 40 kilograms of methyl alcohol, with nitrogen replacement reactive system three times, then blow three times with hydrogen, then close relief valve, open hydrogen gas valve, until autoclave internal pressure reaches 0.15MPa.Close intake valve, be then heated to 32 DEG C ± 2 DEG C, and insulation reaction 4 hours at this temperature, supplement logical hydrogen twice in the middle of this process needs, till reaction no longer absorbs hydrogen.Cooling, release, by reacting liquid filtering, reclaims catalyzer, then by upper for filtrate tower rectifying, isolates desired product 2-methyl butanol 19.2 kilograms, GC content 99.5%, yield 91.7%.
embodiment 3:
20 kilograms of 2-ethyl acrylic aldehyde, Raney's nickel, 50 kilograms of ethyl acetate are added successively in the autoclave of 100L, with nitrogen replacement reactive system three times, then blow three times with hydrogen, then close relief valve, open hydrogen gas valve, until autoclave internal pressure reaches 0.9MPa.Close intake valve, be then heated to 65 DEG C ± 2 DEG C, and insulation reaction 5 hours at this temperature, supplement logical hydrogen twice in the middle of this process needs, till reaction no longer absorbs hydrogen.Cooling, release, by reacting liquid filtering, reclaims catalyzer, then by upper for filtrate tower rectifying, isolates desired product 2-methyl butanol 20.1 kilograms, GC content 99.8%, yield 96.0%.
Claims (6)
1. a preparation method for 2-methyl butanol, is characterized in that comprising the steps and processing condition:
(1) in autoclave, drop into 2-ethyl acrylic aldehyde, catalysts and solvents, adopt nitrogen replacement reaction system, then blow three times with hydrogen, then close relief valve, be filled with hydrogen in still, pressure-controlling is at 0.1-1MPa;
(2) reaction at temperature control 0-80 DEG C, still internal pressure carries out reduction reaction at 0.1-1MPa, insulation reaction 3-5 hour;
(3) after above-mentioned (2) have reacted, filtering recovering catalyst, reusable edible 5-8 time;
(4) filtrate of above-mentioned (3) is transferred to rectifying tower, obtains product after rectifying, yield 85-98%, GC >=99.5%.
2. the preparation method of a kind of 2-methyl butanol according to claim 1, is characterized in that: described catalyzer is platinum carbon or Raney's nickel.
3. the preparation method of a kind of 2-methyl butanol according to claim 1, is characterized in that: described solvent is methyl alcohol, ethanol, Virahol, ethyl acetate or tetrahydrofuran (THF).
4. the preparation method of a kind of 2-methyl butanol according to claim 1, is characterized in that: 2-ethyl acrylic aldehyde, catalyst weight are than being 1:0.01-0.1.
5. the preparation method of a kind of 2-methyl butanol according to claim 1, is characterized in that: described reduction reaction temperature 0-80 DEG C.
6. the preparation method of a kind of 2-methyl butanol according to claim 1, is characterized in that: described reacting kettle inner pressure is at 0.1-1MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510484045.5A CN105001057B (en) | 2015-08-10 | 2015-08-10 | Preparation method of 2-methylbutanol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510484045.5A CN105001057B (en) | 2015-08-10 | 2015-08-10 | Preparation method of 2-methylbutanol |
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| CN105001057A true CN105001057A (en) | 2015-10-28 |
| CN105001057B CN105001057B (en) | 2017-05-03 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4968849A (en) * | 1988-02-05 | 1990-11-06 | Huels Aktiengesellschaft | Process for the preparation of 2-ethylhexanol by liquid-phase catalytic hydrogenation of 2-ethylhexenal, and catalyst |
| CN104119204A (en) * | 2014-07-24 | 2014-10-29 | 刘琴 | Hydrogenation method of octenal |
| CN104140358A (en) * | 2014-07-28 | 2014-11-12 | 万华化学集团股份有限公司 | Method for preparing trimethylolpropane through hydrogenation |
-
2015
- 2015-08-10 CN CN201510484045.5A patent/CN105001057B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4968849A (en) * | 1988-02-05 | 1990-11-06 | Huels Aktiengesellschaft | Process for the preparation of 2-ethylhexanol by liquid-phase catalytic hydrogenation of 2-ethylhexenal, and catalyst |
| CN104119204A (en) * | 2014-07-24 | 2014-10-29 | 刘琴 | Hydrogenation method of octenal |
| CN104140358A (en) * | 2014-07-28 | 2014-11-12 | 万华化学集团股份有限公司 | Method for preparing trimethylolpropane through hydrogenation |
Non-Patent Citations (2)
| Title |
|---|
| 崔文峰等: "2-甲基丁醇的合成与应用研究进展", 《精细石油化工》 * |
| 张涛等: "镍基催化剂上2-丙基-2-庚烯醛液相加氢工艺研究", 《石油化工》 * |
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Denomination of invention: A preparation method of 2-methylbutanol Effective date of registration: 20230228 Granted publication date: 20170503 Pledgee: China CITIC Bank Co.,Ltd. Xiangyang Branch Pledgor: HUBEI JINGHONG CHEMICAL Co.,Ltd. Registration number: Y2023980033561 |
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