CN106631783A - Preparation method for n-butyl acetate - Google Patents
Preparation method for n-butyl acetate Download PDFInfo
- Publication number
- CN106631783A CN106631783A CN201610901932.2A CN201610901932A CN106631783A CN 106631783 A CN106631783 A CN 106631783A CN 201610901932 A CN201610901932 A CN 201610901932A CN 106631783 A CN106631783 A CN 106631783A
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- China
- Prior art keywords
- butyl acetate
- preparation
- water
- acetic acid
- catalyst
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/053—Sulfates
Abstract
The invention relates to a preparation method for n-butyl acetate. The method comprises the following steps: taking a self-prepared solid super acid as a catalyst; taking acetic acid and n-butyl alcohol as reaction raw materials; and refluxing and separating water, thereby acquiring n-butyl acetate. The self-prepared catalyst is a solid super acid which is prepared in the manner of taking ammonium ferric sulfate residue after catalytic esterification reaction as the raw material and roasting by a muffle furnace. According to the invention, the ammonium ferric sulfate residue after catalytic esterification reaction is reused, the emission of the solid waste is reduced and the benefit in environmental protection is excellent. Meanwhile, the catalyst prepared according to the method has the advantages of excellent catalytic activity, high selectivity, reusability, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of n-butyl acetate, more particularly to a kind of in self-control solid superacid as catalyst
The method that the lower acetic acid of agent effect prepares n-butyl acetate with n-butanol reaction.
Background technology
N-butyl acetate is a kind of water white flammable liquid, the fruit aroma with slightly below pentyl acetate.It
Can dissolve each other with the conventional organic solvent of alcohol, ketone, ester and great majority.In addition, although n-butyl acetate have anesthesia and stimulation, but
Its acute toxicity is less.Therefore, n-butyl acetate as organic solvent, extractant or dehydrating agent etc. and can be applied to varnish, people
It is that a kind of important basic organic chemical industry is former in the industrial productions such as fabricate-leather, nitrocellulose, medicine, collodion, spices and plastics
Material.
At present, the key industry production method of n-butyl acetate is sulphate method.The method with the concentrated sulfuric acid as catalyst, with second
Acid is raw material with n-butanol, by gap operating or continuous operation production n-butyl acetate.Although the method has technical maturity, sets
Standby simple and easy to operate the advantages of, but due to the use of the concentrated sulfuric acid being catalyst, there is following defect in this method：1. n-butyl acetate
Poor selectivity, refine difficulty：The concentrated sulfuric acid while catalytic esterification, also can catalysis oxidation, dehydration, sulfonation, charing and
The reaction such as polymerization；2. the recycling of raw material is more difficult；3. the separation of catalyst is difficult：Need the neutralization of Jing alkali, washing etc. follow-up
Operation, causes n-butyl acetate that a large amount of waste water are produced while loss；4. the concentrated sulfuric acid is serious to equipment corrosion, causes equipment investment
Greatly, production cost is high.
In view of sulphate method produces the subject matter that n-butyl acetate is present, many researchers are just being devoted to correlation and are grinding
Study carefully, emerged in large numbers large quantities of new catalysts, such as lewis acid, sulfamic acid, sulfonate resin, solid super-strong acid, heteropoly acid etc.,
Different degrees of solves problem above.Researcher just once using ammonium ferric sulfate had synthesized n-butyl acetate for catalyst,
But the ammonium ferric sulfate effect waste discharge after use, to environmental protection certain pressure is also brought.
The content of the invention
For the deficiencies in the prior art, the present invention is intended to provide a kind of ammonium ferric sulfate waste residue with after catalytic esterification is
Raw material, prepares solid super-strong acid, and as catalyst, high selectivity, the side for preparing n-butyl acetate in high yield, inexpensive
Method.
A kind of preparation method of n-butyl acetate, is anti-with acetic acid and n-butanol to make solid super-strong acid by oneself as catalyst
Raw material is answered, through reflux water-dividing n-butyl acetate is obtained, comprised the following steps：
（1）Prepare catalyst：After for the drying of 12 water and ammonium ferric sulfate, the grinding after catalytic esterification, loaded on crucible,
Put Muffle kiln roasting into, then place roars of laughter in drier and be cooled to room temperature, it is standby；
（2）Thermometer and water knockout drum are respectively mounted on dry there-necked flask, reflux condensing tube is carried on water knockout drum；Thereto
Acetic acid, n-butanol are added, to be started and add step after stirring（1）Gained solid super acid catalyst, is heated, temperature control with electric jacket
At 120 DEG C or so, backflow, point water keeps water layer liquid level in water knockout drum to be less than organic layer liquid level 0.5 to system during Fen Shui
Mm, so as in organic layer energy Returning reactor, react fully；After reaction terminates, sampling carries out makings analysis, and selective 99%
More than, carry out vacuum distillation and collect product, obtain final product.
A kind of preparation method of above-mentioned n-butyl acetate, preferred scheme is, step（1）Sintering temperature is 400-600 DEG C,
It is preferred that 550 DEG C.
A kind of preparation method of above-mentioned n-butyl acetate, preferred scheme is, step（1）Roasting time is 2-8h, preferably
5h。
A kind of preparation method of above-mentioned n-butyl acetate, preferred scheme is, step（2）The consumption of described catalyst is
The 5%-20% of quality of acetic acid, preferably 14%.
A kind of preparation method of above-mentioned n-butyl acetate, preferred scheme is, in step（2）Described acetic acid and n-butanol
Material amount ratio be 1:1-3, preferably 1:1.5.
A kind of preparation method of above-mentioned n-butyl acetate, preferred scheme is, step（2）The acetic acid is anti-with n-butanol
It is 30-120min, preferred 60min between seasonable.
Compared with prior art, the maximum superiority of the present invention is just belonging to twice laid, with catalytic esterification after 12
Water and ammonium ferric sulfate reduce the discharge of solid waste, with good environmental benefit as catalyst preparation materials；Simultaneously
The advantages of catalyst prepared by the method also possesses good catalysis activity, selective height, can be recycled multiple, with fresh 12
The catalyst performance that water and ammonium ferric sulfate roasting are obtained is basically identical.
Specific embodiment：
The present invention is to make solid super-strong acid by oneself as catalyst, there is provided a kind of preparation method of n-butyl acetate, wherein solid surpass
The preparation technology route of strong acid is shown below：
The present invention is further described by the following embodiment, and these descriptions are not to make further to present invention
Limit.It should be understood by those skilled in the art that the equivalent that the technical characteristic of the present invention is made, or be correspondingly improved, still
Belong within protection scope of the present invention.
Embodiment 1
Thermometer and water knockout drum are respectively mounted on 500 dry mL there-necked flasks, reflux condensing tube is carried on water knockout drum.To
Wherein add acetic acid 60g（1mol）, n-butanol 74g（1mol）, start stirring after add 550 DEG C of roasting 2h solid super-strong acid urge
Agent 12g（Account for quality of acetic acid 20%）, being heated with electric jacket, at 120 DEG C or so, backflow, point water is dividing a water process to temperature control
Water layer liquid level is less than the mm of organic layer liquid level 0.5 so as in organic layer energy Returning reactor, fill reaction in middle holding water knockout drum
Point.After reaction 120min, sampling carries out makings analysis, and selective more than 99%, carry out vacuum distillation and collect product, yield 92%,
Content 99%.
Embodiment 2
Thermometer and water knockout drum are respectively mounted on 500 dry mL there-necked flasks, reflux condensing tube is carried on water knockout drum.To
Wherein add acetic acid 60g（1mol）, n-butanol 111g（1.5mol）, start the solid super strong that 550 DEG C of roasting 5h are added after stirring
Acid catalyst 8.4g（Account for quality of acetic acid 14%）, being heated with electric jacket, at 120 DEG C or so, backflow, point water is dividing temperature control
Water layer liquid level in water knockout drum is kept to be less than the mm of organic layer liquid level 0.5 during water so as in organic layer energy Returning reactor, make anti-
Should be abundant.After reaction 60min, sampling carries out makings analysis, and selective more than 99%, carry out vacuum distillation and collect product, yield
99%, content 99%.
Embodiment 3
Thermometer and water knockout drum are respectively mounted on 500 dry mL there-necked flasks, reflux condensing tube is carried on water knockout drum.To
Wherein add acetic acid 60g（1mol）, n-butanol 222g（3mol）, start the solid super-strong acid that 600 DEG C of roasting 4h are added after stirring
Catalyst 3g（Account for quality of acetic acid 5%）, being heated with electric jacket, at 120 DEG C or so, backflow, point water is dividing a water process to temperature control
Water layer liquid level is less than the mm of organic layer liquid level 0.5 so as in organic layer energy Returning reactor, fill reaction in middle holding water knockout drum
Point.After reaction 30min, sampling carries out makings analysis, and selective more than 99%, carry out vacuum distillation and collect product, yield 94% contains
Amount 99%.
Embodiment 4
Thermometer and water knockout drum are respectively mounted on 500 dry mL there-necked flasks, reflux condensing tube is carried on water knockout drum.To
Wherein add acetic acid 60g（1mol）, n-butanol 111g（1.5mol）, start the solid super strong that 400 DEG C of roasting 8h are added after stirring
Acid catalyst 12g（Account for quality of acetic acid 20%）, being heated with electric jacket, at 120 DEG C or so, backflow divides water, in Fen Shui to temperature control
During keep water knockout drum in water layer liquid level less than the mm of organic layer liquid level 0.5 so as in organic layer energy Returning reactor, make reaction
Fully.After reaction 120min, sampling carries out makings analysis, and selective more than 99%, carry out vacuum distillation and collect product, yield
95%, content 99%.
Embodiment 5
Thermometer and water knockout drum are respectively mounted on 500 dry mL there-necked flasks, reflux condensing tube is carried on water knockout drum.To
Wherein add acetic acid 60g（1mol）, n-butanol 222g（3mol）, start the solid super-strong acid that 500 DEG C of roasting 4h are added after stirring
Catalyst 6g（Account for quality of acetic acid 10%）, being heated with electric jacket, at 120 DEG C or so, backflow, point water is dividing a water mistake to temperature control
Water layer liquid level in water knockout drum is kept to be less than the mm of organic layer liquid level 0.5 so as in organic layer energy Returning reactor, fill reaction in journey
Point.After reaction 90min, sampling carries out makings analysis, and selective more than 99%, carry out vacuum distillation and collect product, yield 97% contains
Amount 99%.
Claims (6)
1. a kind of preparation method of n-butyl acetate, it is characterised in that to make solid super-strong acid by oneself as catalyst, with acetic acid and just
Butanol is reaction raw materials, and through reflux water-dividing n-butyl acetate is obtained, and is comprised the following steps：
（1）Prepare catalyst：After for the drying of 12 water and ammonium ferric sulfate, the grinding after catalytic esterification, loaded on crucible,
Put Muffle kiln roasting into, then place roars of laughter in drier and be cooled to room temperature, it is standby；
（2）Thermometer and water knockout drum are respectively mounted on dry there-necked flask, reflux condensing tube is carried on water knockout drum；Thereto
Acetic acid, n-butanol are added, to be started and add step after stirring（1）Gained solid super acid catalyst, is heated, temperature control with electric jacket
At 120 DEG C or so, backflow, point water keeps water layer liquid level in water knockout drum to be less than organic layer liquid level 0.5 to system during Fen Shui
Mm, so as in organic layer energy Returning reactor, react fully；After reaction terminates, sampling carries out makings analysis, and selective 99%
More than, carry out vacuum distillation and collect product, obtain final product.
2. a kind of preparation method of n-butyl acetate according to claim 1, it is characterised in that step（1）Sintering temperature
For 400-600 DEG C, preferably 550 DEG C.
3. a kind of preparation method of n-butyl acetate according to claim 1, it is characterised in that step（1）Roasting time
For 2-8h, preferred 5h.
4. a kind of preparation method of n-butyl acetate according to claim 1, it is characterised in that step（2）Described urges
The consumption of agent for quality of acetic acid 5%-20%, preferably 14%.
5. the preparation method of a kind of n-butyl acetate according to claim 1, it is characterised in that in step（2）Described
Acetic acid is 1 with the amount ratio of the material of n-butanol:1-3, preferably 1:1.5.
6. a kind of preparation method of n-butyl acetate according to claim 1, it is characterised in that step（2）The acetic acid
It is 30-120min, preferred 60min with the reaction time of n-butanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610901932.2A CN106631783A (en) | 2016-10-18 | 2016-10-18 | Preparation method for n-butyl acetate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610901932.2A CN106631783A (en) | 2016-10-18 | 2016-10-18 | Preparation method for n-butyl acetate |
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| CN106631783A true CN106631783A (en) | 2017-05-10 |
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| CN201610901932.2A Pending CN106631783A (en) | 2016-10-18 | 2016-10-18 | Preparation method for n-butyl acetate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017538A (en) * | 2017-12-25 | 2018-05-11 | 荆州市江汉精细化工有限公司 | A kind of preparation method of n-butyl acetate |
| CN109550507A (en) * | 2018-12-07 | 2019-04-02 | 徐州伯利恒生物科技有限公司 | A kind of synthetic method of butyl glycolate |
| CN115608410A (en) * | 2021-07-13 | 2023-01-17 | 中国石油化工股份有限公司 | Catalyst for synthesizing n-butyl acetate and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020631A (en) * | 2007-03-23 | 2007-08-22 | 上海工程技术大学 | S2O8 2-/TiO2 Al2 O3 super solid acid catalyzed n-butyl acetate synthesizing process |
-
2016
- 2016-10-18 CN CN201610901932.2A patent/CN106631783A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020631A (en) * | 2007-03-23 | 2007-08-22 | 上海工程技术大学 | S2O8 2-/TiO2 Al2 O3 super solid acid catalyzed n-butyl acetate synthesizing process |
Non-Patent Citations (2)
| Title |
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| 于龙 等: "固体超强酸SO42-/Fe2O3催化合成尼泊金丁酯", 《食品工业科技》 * |
| 孔祥文、于龙: "固体超强酸SO42-/Fe2O3催化合成乙酸正丁酯", 《实验技术与管理》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017538A (en) * | 2017-12-25 | 2018-05-11 | 荆州市江汉精细化工有限公司 | A kind of preparation method of n-butyl acetate |
| CN109550507A (en) * | 2018-12-07 | 2019-04-02 | 徐州伯利恒生物科技有限公司 | A kind of synthetic method of butyl glycolate |
| CN115608410A (en) * | 2021-07-13 | 2023-01-17 | 中国石油化工股份有限公司 | Catalyst for synthesizing n-butyl acetate and preparation method and application thereof |
| CN115608410B (en) * | 2021-07-13 | 2023-10-13 | 中国石油化工股份有限公司 | Catalyst for synthesizing n-butyl acetate and preparation method and application thereof |
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Application publication date: 20170510 |