CN102731298A - Method for purifying ethyl acetate - Google Patents
Method for purifying ethyl acetate Download PDFInfo
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- CN102731298A CN102731298A CN2012102524163A CN201210252416A CN102731298A CN 102731298 A CN102731298 A CN 102731298A CN 2012102524163 A CN2012102524163 A CN 2012102524163A CN 201210252416 A CN201210252416 A CN 201210252416A CN 102731298 A CN102731298 A CN 102731298A
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- ethyl acetate
- ethyle acetate
- potassium carbonate
- molecular sieve
- calcium chloride
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Abstract
The invention discloses a method for purifying ethyl acetate, which comprises the steps of: sequentially adding 4-6wt% sodium sulfite solution and saturated calcium chloride solution into industrial-grade ethyl acetate serving as a raw material; stirring to remove organic impurities in ethyl acetate; then sequentially adding anhydrous potassium carbonate for drying and 4A molecular sieve for adsorbing and purifying; and finally collecting purified ethyl acetate by a rectification method, wherein the purity of ethyl acetate purified by the method is more than 99.5%. Compared with the prior art, the method is safe, simple and convenient in the purification process, and can save energy and reduce emission; after being treated, the added purifying agent can be recycled, so that the method is in accordance with the requirements of green chemical industry and environmental protection; and the ethyl acetate product purified by the method is stable in quality and high in purity, and has the prospect of industrial production.
Description
Technical field
The present invention relates to a kind of purification process of ETHYLE ACETATE, particularly a kind of massfraction that uses is the method for 4～6% sodium sulfite solution, saturated calcium chloride solution, Anhydrous potassium carbonate and 4A molecular sieve purification purifying ethyl acetate.
Background technology
ETHYLE ACETATE is colourless transparent liquid, has fruit fragrant, volatile, to air-sensitive, can absorb water and divide, and moisture can make it slowly decompose and be acid.Can be miscible with chloroform, ethanol, acetone and ether, water-soluble (10ml/ml).Can dissolve some metallic salt (like lithium chloride, NSC 51149, zinc chloride, iron(ic)chloride etc.).Specific density is 0.902, and fusing point is-83 ℃, and boiling point is 77 ℃, and refractive index is 1.3719, and flash-point is 7.2 ℃ (opening cup).Inflammable, steam can form explosive mixture with air.Pungency is arranged, medium lethal dose(LD&-{50}) (rat, per os) 11.3ml/kg.As extraction agent, can from the aqueous solution, extract chemical compound lot (phosphorus, tungsten, arsenic, cobalt).Can be used as the reference material of Tc meter when separating carbohydrate.Calibrating bismuth, gold, iron, mercury, oxygenant and platinum.Measure bismuth, boron, gold, iron, molybdenum, platinum, potassium and thallium.Be used for Biochemical Research, protein sequencing, pesticide residue analysis.Be used for organic synthesis, the spices manufacturing, can do using wine blending spices, artificial essence, TKK 021, nitrocellulose, xylonite, varnish, coating, leatheroid, malthoid, regenerated fiber, printing-ink etc.Also can make the raw material of sticker, medicine and organic acid extraction agent and the fruity perfume of olivet.
Its structural formula of ETHYLE ACETATE is following:
In the prior art, very few to the research disclosure of ETHYLE ACETATE method of purification.Because major impurity is multiple organism such as water, acetate, alcohol in the industrial goods ETHYLE ACETATE; Conventional method of purification is to adopt air distillation to obtain the purified acetic acid ethyl ester with anhydrous calciumsulphate dehydration back earlier; Though this method purification step is easy; But the product that obtains with this method purification can't reach industry standard, does not have the prospect of industrialization; Chinese patent CN201110005871.9 discloses a kind of purification process of ETHYLE ACETATE, and this method obtains ethyl acetate product with the purifying mixture of ethyl acetate, alcohol and water.Which comprises at least ETHYLE ACETATE rectifying tower, ETHYLE ACETATE regenerating column and ethanol regenerating column and support equipment thereof.Heat is integrated between ETHYLE ACETATE rectifying tower, the ETHYLE ACETATE regenerating column, obtains ethyl acetate product by ETHYLE ACETATE rectifying Tata still.It is extraction agent that the ETHYLE ACETATE regenerating column adopts water, carries out the extracting rectifying operation, recovered overhead ETHYLE ACETATE, and tower still discharging ethanol-water mixture removes the ethanol regenerating column.Ethanol reclaims the Tata still and obtains ethanol-water mixture, and a tower still waste water part recycles, and other dischargings, goes out device.Add that other heat exchange in the system, energy-conservation application have greatly reduced operation energy consumption.Operation energy consumption of the present invention is reduced to 0.55 ton of steam/ton ethyl acetate product, and the ETHYLE ACETATE process for purification cuts down the consumption of energy more than 50% at present, adds that no ETHYLE ACETATE returns reaction process; Can make the reaction process energy consumption reduce more than 30%; The product purity that this method obtains is high, but complex steps, and the time is long; Cost is high, and the value of suitability for industrialized production is little.
Summary of the invention
Technical problem to be solved by this invention provides a kind of purification process of ETHYLE ACETATE, and is low to overcome in the prior art ETHYLE ACETATE purified product purity, complex operation step, and the time is long, the deficiency that cost is high.
Technical conceive of the present invention is such:
The present invention is a raw material with technical grade ETHYLE ACETATE; Adding massfraction successively is 4～6% sodium sulfite solutions and saturated calcium chloride solution; Stirring is to remove the organic impurity in the ETHYLE ACETATE; Add successively again that Anhydrous potassium carbonate carries out drying and the 4A molecular sieve carries out adsorption and purification, adopt rectificating method to collect at last and obtain the purified acetic acid ethyl ester.
Technical scheme of the present invention:
With massfraction is that 4～6% sodium sulfite solution and saturated calcium chloride solution add in the ETHYLE ACETATE successively; Stir 10～20min; Add Anhydrous potassium carbonate then; Reflux 1～2h adds the 4A molecular sieve again and carries out adsorption and purification 20～30min, and last flow velocity with 10-20mL/min carries out rectified and collected and obtains the purified acetic acid ethyl ester.
According to the present invention, described ETHYLE ACETATE and massfraction are that the volume ratio of 4～6% sodium sulfite solution is 1:0.02～0.03, ml/mL; The volume ratio of described ETHYLE ACETATE and saturated calcium chloride solution is 1:0.01～0.02, ml/mL; Described ETHYLE ACETATE is 1:0.05～0.07, ml/g with the volume mass ratio of Anhydrous potassium carbonate; Described ETHYLE ACETATE is 1:0.04～0.06, ml/g with the volume mass ratio of 4A molecular sieve.
The primary industry article ETHYLE ACETATE that the present invention is used; Purifying agent S-WAT, calcium chloride, Anhydrous potassium carbonate, 4A molecular sieve all have sale on market; Raw material is easy to get; Employed purifying agent can recycle after treatment, and the ETHYLE ACETATE purity that obtains with purification process of the present invention is greater than 99.5%.
Beneficial effect of the present invention:
1. the massfraction of the present invention's employing is 4～6% sodium sulfite solution, saturated calcium chloride solution, Anhydrous potassium carbonate, 4A molecular sieve, can effectively remove the impurity in the raw acetic acid ethyl ester, and purge process is safe and simple, energy-saving and emission-reduction;
2. used Anhydrous potassium carbonate, the 4A molecule sieve after being treated of the present invention can recycle, and meets green chemical industry, the protection environment requirement;
3. purification process yield of the present invention is high, the ethyl acetate product steady quality of acquisition, and purity is high, has industrial production foreground.
Embodiment
Through embodiment the present invention is described further below, but embodiment does not limit protection scope of the present invention.
Embodiment 1
1000ml industrial goods ETHYLE ACETATE is joined 2000ml to be had in the there-necked flask of rectifier unit, TM, heating and whipping appts; Add massfraction successively and be 4% sodium sulfite solution 20ml and saturated calcium chloride solution 10ml; Stir 10min to remove the organic impurity in the ETHYLE ACETATE, add Anhydrous potassium carbonate 50g then, reflux 1h; Add the 40g4A molecular sieve again and carry out adsorption and purification 20min; Last flow velocity with 20mL/min carries out rectified and collected and obtains purified acetic acid ethyl ester 907ml, and yield is 90.7%, and purity is 99.53%.
Embodiment 2
1000ml industrial goods ETHYLE ACETATE is joined 2000ml to be had in the there-necked flask of rectifier unit, TM, heating and whipping appts; Add massfraction successively and be 5% sodium sulfite solution 25ml and saturated calcium chloride solution 15ml; Stir 15min to remove the organic impurity in the ETHYLE ACETATE, add Anhydrous potassium carbonate 60g then, reflux 1.5h; Add the 50g4A molecular sieve again and carry out adsorption and purification 25min; Last flow velocity with 15mL/min carries out rectified and collected and obtains purified acetic acid ethyl ester 919ml, and yield is 91.9%, and purity is 99.78%.
Embodiment 3
1000ml industrial goods ETHYLE ACETATE is joined 2000ml to be had in the there-necked flask of rectifier unit, TM, heating and whipping appts; Add massfraction successively and be 6% sodium sulfite solution 30ml and saturated calcium chloride solution 20ml; Stir 20min to remove the organic impurity in the ETHYLE ACETATE, add Anhydrous potassium carbonate 70g then, reflux 2h; Add the 60g4A molecular sieve again and carry out adsorption and purification 30min; Last flow velocity with 10mL/min carries out rectified and collected and obtains purified acetic acid ethyl ester 927ml, and yield is 92.7%, and purity is 99.91%.
Need to prove that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is specified with reference to preferred embodiment; Those of ordinary skill in the art is to be understood that; Can make amendment or be equal to replacement the technical scheme of invention, and not break away from the scope of technical scheme of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (6)
1. the purification process of an ETHYLE ACETATE; It is characterized in that, comprise the steps: with massfraction to be that 4～6% sodium sulfite solution and saturated calcium chloride solution add in the ETHYLE ACETATE successively, stir 10～20min; Add Anhydrous potassium carbonate then; Reflux 1～2h adds the 4A molecular sieve again and carries out adsorption and purification 20～30min, and last flow velocity with 10-20mL/min carries out rectified and collected and obtains the purified acetic acid ethyl ester.
2. method according to claim 1 is characterized in that, described ETHYLE ACETATE and massfraction are that the volume ratio of 4～6% sodium sulfite solution is 1:0.02～0.03, ml/mL.
3. method according to claim 1 is characterized in that, the volume ratio of described ETHYLE ACETATE and saturated calcium chloride solution is 1:0.01～0.02, ml/mL.
4. method according to claim 1 is characterized in that, described ETHYLE ACETATE is 1:0.05～0.07, ml/g with the volume mass ratio of Anhydrous potassium carbonate.
5. method according to claim 1 is characterized in that, described ETHYLE ACETATE is 1:0.04～0.06, ml/g with the volume mass ratio of 4A molecular sieve.
6. method according to claim 1 is characterized in that: the purity of described S-WAT, calcium chloride, Anhydrous potassium carbonate and 4A molecular sieve is analytical pure.
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| CN2012102524163A CN102731298A (en) | 2012-07-20 | 2012-07-20 | Method for purifying ethyl acetate |
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| CN2012102524163A CN102731298A (en) | 2012-07-20 | 2012-07-20 | Method for purifying ethyl acetate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104693028A (en) * | 2015-03-31 | 2015-06-10 | 太仓沪试试剂有限公司 | Purification method of ethyl acetate |
| CN104903364A (en) * | 2012-12-20 | 2015-09-09 | 巴塞尔聚烯烃股份有限公司 | Process for copolymerizing ethylene and esters of vinyl alcohol |
| CN105085260A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of ethyl acetate for liquid chromatography-mass spectrometer |
| CN105622415A (en) * | 2016-02-18 | 2016-06-01 | 国药集团化学试剂有限公司 | Ethyl acetate quality improving method |
| RU2604235C2 (en) * | 2015-01-28 | 2016-12-10 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Method of producing pellet powder for small arms cartridges |
| CN107324995A (en) * | 2017-08-29 | 2017-11-07 | 湖北工程学院 | A kind of chromatogram pure ethyl acetate and preparation method thereof, production system |
Citations (2)
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| JPS5781436A (en) * | 1980-11-10 | 1982-05-21 | Tokuyama Sekiyu Kagaku Kk | Purification of ethyl acetate |
| CN102070444A (en) * | 2010-12-21 | 2011-05-25 | 东莞市杉杉电池材料有限公司 | Ethyl acetate dehydration and impurity removing method |
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2012
- 2012-07-20 CN CN2012102524163A patent/CN102731298A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5781436A (en) * | 1980-11-10 | 1982-05-21 | Tokuyama Sekiyu Kagaku Kk | Purification of ethyl acetate |
| CN102070444A (en) * | 2010-12-21 | 2011-05-25 | 东莞市杉杉电池材料有限公司 | Ethyl acetate dehydration and impurity removing method |
Non-Patent Citations (2)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104903364A (en) * | 2012-12-20 | 2015-09-09 | 巴塞尔聚烯烃股份有限公司 | Process for copolymerizing ethylene and esters of vinyl alcohol |
| CN104903364B (en) * | 2012-12-20 | 2017-12-05 | 巴塞尔聚烯烃股份有限公司 | The method being copolymerized for the esters for making ethene and vinyl alcohol |
| US10005862B2 (en) | 2012-12-20 | 2018-06-26 | Basell Polyolefine Gmbh | Process for copolymerizing ethylene and esters of vinyl alcohol |
| CN105085260A (en) * | 2014-05-16 | 2015-11-25 | 上海星可高纯溶剂有限公司 | Purification method of ethyl acetate for liquid chromatography-mass spectrometer |
| RU2604235C2 (en) * | 2015-01-28 | 2016-12-10 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических продуктов" (ФКП "ГосНИИХП") | Method of producing pellet powder for small arms cartridges |
| CN104693028A (en) * | 2015-03-31 | 2015-06-10 | 太仓沪试试剂有限公司 | Purification method of ethyl acetate |
| CN105622415A (en) * | 2016-02-18 | 2016-06-01 | 国药集团化学试剂有限公司 | Ethyl acetate quality improving method |
| CN107324995A (en) * | 2017-08-29 | 2017-11-07 | 湖北工程学院 | A kind of chromatogram pure ethyl acetate and preparation method thereof, production system |
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Application publication date: 20121017 |