CN104744198A - Method for preparing ethylene in laboratory - Google Patents
Method for preparing ethylene in laboratory Download PDFInfo
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- CN104744198A CN104744198A CN201510134325.3A CN201510134325A CN104744198A CN 104744198 A CN104744198 A CN 104744198A CN 201510134325 A CN201510134325 A CN 201510134325A CN 104744198 A CN104744198 A CN 104744198A
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Abstract
The invention discloses a method for preparing ethylene in a laboratory. Two liquid reagents, namely 95% ethanol and concentrated sulfuric acid in the laboratory are completely absorbed with solid powder; the experiment is changed into a solid reagent from the liquid reagent; a heated generator is changed into an ordinary large test tube from a flask or a distillation flask; and a thermometer does not need to be arranged. The yield of the ethylene prepared by the method disclosed by the invention is over 90%, and is improved by more than twice; after the experiment is ended, reaction residues (recoverable) are poured and no carbon granule is adhered to the inner wall of the test tube; and the test tube can be washed only by running water. The prepared ethylene is obvious in phenomenon in a property test, and is used for preparing synthetic 1,2-dibromoethane; and a god effect is also obtained.
Description
Technical field
The present invention relates to Basic experimental teaching technical field, particularly relate to a kind of method of Preparing Ethylene in Lab.
Background technology
The preparation experiment of ethene is an important infrastest in senior chemistry textbook (second) and Experimental Organic Chemistry in Colleges teaching material.The traditional method of Preparing Ethylene in Lab is the mixture heat altogether utilizing the vitriol oil (catalyzer) and ethanol.Catalyzer is made with the vitriol oil, cheap and easy to get, can experimental cost be reduced, but it also brings this experiment at least to there are following 3 deficiencies: (1) dense H
2sO
4consumption large, specific heat is high again, and the time be heated to needed for 170 DEG C is longer, and difficult control of temperature.(2) because the strong oxidizing property of the vitriol oil and ethanol easily carbonize, the ethylene yield obtained is low, and purity is not high, is mixed with more CO
2, SO
2, CO, the gas (wherein the volume of first two gas accounts for 1/3 of volume of gas) such as ether, not only have impact on the verity of experimental phenomena, and cause the severe contamination of laboratory or Classroom air.(3) the serious charing of ethanol makes to react mixture in rear flask is brownish black, and carbon deposit invests a bottle wall and is difficult to cleaning.Therefore, how improving output and the purity of ethene, be not only the important Teaching subject in basic education field, is also an important research direction of experimental technique.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of Preparing Ethylene in Lab.By highlighting the catalytic of the vitriol oil, weaken the oxidisability of the vitriol oil, thus reach the object improving ethylene yield and purity.
The present invention adopts following technical scheme:
The method of Preparing Ethylene in Lab of the present invention is all absorbed 95% ethanol in experiment and the vitriol oil two kinds of liquid reagent pressed powders, experiment is become " solid reagent " from liquid reagent, also changed into common Boiling tube by flask or distilling flask by the producer heated, and do not need thermometer is installed.
The concrete steps of method of the present invention are as follows:
(1) 95% ethanol is mixed with the volume ratio of the vitriol oil by 1:3, make alkyd mixed solution, placed through 6-12 hour, make ethanol fully obtain esterification and generate vinic acid;
(2) take the pressed powder of mixing, pour in beaker, then measure the good alkyd mixed solution of esterification prepared by step (1) with graduated cylinder, also pour into wherein, then mix thoroughly, every 10-15g pressed powder adds 10ml alkyd mixed solution;
(3) the blended solid powder absorbing alkyd mixed solution mixed thoroughly is encased in Boiling tube, and the single hole soft rubber ball got ready in advance beyond the Great Wall, the mode of conveniently solid heating fixes device, can carry out producing and relevant property test of ethene.
Described pressed powder is the mixture of coal ash of anhydrous sulfate, metal oxide and drying, and its weight ratio is followed successively by 5-10 part; 0.1-1 part; 1-5 part.
As one of preferred technical scheme: described pressed powder consist of anhydrous slufuric acid calcium powder 7 weight part, lime powder 0.5 weight part, dry coal ash 2.5 weight part.
As preferred technical scheme two: described pressed powder consist of anhydrous slufuric acid magnesium dust 6 weight part, magnesium oxide 0.35 weight part, dry coal ash 3.65 weight part.
As preferred technical scheme three: described pressed powder consist of anhydrous slufuric acid zinc powder 5 weight part, Zinc oxide powder 0.5 weight part, dry coal ash 4.5 weight part.
Described coal ash is the cinder ash from the drying of boiler house, obtains through 100 mesh sieve.
Positively effect of the present invention is as follows:
In traditional ethylene making process, along with the rising of temperature of reaction, in system, the amount of second alcohol and water constantly reduces, and the concentration of the vitriol oil can be increasing, its dehydration and oxygenizement also more and more stronger.And in this experiment, can not flow arbitrarily in certain position that the vitriol oil is fixedly secured to pressed powder, have to " lying up " after having participated in dehydration reaction, and the unnecessary vitriol oil of part " is eaten up " by the metal oxide of aobvious alkalescence again.Thus the ethanol that sulfuric acid concentration can be reduced to raise and cause is oxidized and the side reaction of charing occurs, thus greatly increase output and the purity of ethene.
The productive rate of method preparing ethylene of the present invention is more than 90%, and comparatively Traditional Method doubles many.Test the complete residue of falling dereaction (recyclable) afterwards inboard wall of test tube adhere to without carbon granules, only need tap water to rinse well.It is fairly obvious that the ethene produced does property experiment phenomenon; For the synthesis of the preparation of glycol dibromide, also achieve good effect.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
(1) 95% ethanol is mixed with the volume ratio of the vitriol oil by 1:3, make alkyd mixed solution.Placed through 6-12 hour, make ethanol fully obtain esterification and generate vinic acid.
(2) take about 13.5g pressed powder A (pressed powder A consists of anhydrous slufuric acid calcium powder 7 weight part, lime powder 0.5 weight part, dry coal ash 2.5 weight part), pour in beaker.
(3) measure 10ml with graduated cylinder and shift to an earlier date the good alkyd mixed solution of esterification.
(4) stir the pressed powder in beaker with glass stick, at leisure the alkyd mixed solution in graduated cylinder is poured into wherein, and constantly stir.Solid powder particle in beaker comparatively disperses but till being still in bond state.
(5) pressed powder absorbing alkyd mixed solution mixed thoroughly is encased in Boiling tube, and is ready in advance beyond the Great Wall and is inserted with the single hole soft rubber ball of conduit.Conveniently the mode of solid heating fixes device.
(6) with spirit lamp, to Boiling tube heating, (note preheating, whole mixt is heated evenly; The spirit lamp that moves around at leisure is needed in heat-processed), in time having gas to generate, as required, available drainage collects the gas of whole bottle; Also gas can be chewed by point and light; Or pass in the carbon tetrachloride solution of bromine or the acidic solution of potassium permanganate, carry out the relevant nature test of ethene.
The productive rate of the present embodiment ethene is 92.5%.When doing relevant nature with it, experimental phenomena is fairly obvious; When preparing glycol dibromide with it, effect is also fine.
Embodiment 2
(1) 95% ethanol is mixed with the volume ratio of the vitriol oil by 1:3, make alkyd mixed solution.Placed through 6-12 hour, make ethanol fully obtain esterification and generate vinic acid.
(2) take about 12g pressed powder B (pressed powder B consists of anhydrous slufuric acid magnesium dust 6 weight part, magnesium oxide 0.35 weight part, dry coal ash 3.65 weight part), pour in beaker.
(3) measure 10ml with graduated cylinder and shift to an earlier date the good alkyd mixed solution of esterification.
(4) stir the pressed powder in beaker with glass stick, at leisure the alkyd mixed solution in graduated cylinder is poured into wherein, and constantly stir.Solid powder particle in beaker comparatively disperses but till being still in bond state.
(5) pressed powder absorbing alkyd mixed solution mixed thoroughly is encased in Boiling tube, and is ready in advance beyond the Great Wall and is inserted with the single hole soft rubber ball of conduit.Conveniently the mode of solid heating fixes device.
(6) with spirit lamp, to Boiling tube heating, (note preheating, whole mixt is heated evenly; The spirit lamp that moves around at leisure is needed in heat-processed), in time having gas to generate, as required, available drainage collects the gas of whole bottle; Also gas can be chewed by point and light; Or pass in the carbon tetrachloride solution of bromine or the acidic solution of potassium permanganate, carry out the relevant nature test of ethene.
The productive rate of the present embodiment ethene is 90.8%.When doing relevant nature with it, experimental phenomena is fairly obvious; When preparing glycol dibromide with it, effect is also fine.
Embodiment 3
(1) 95% ethanol is mixed with the volume ratio of the vitriol oil by 1:3, make alkyd mixed solution.Placed through 6-12 hour, make ethanol fully obtain esterification and generate vinic acid.
(2) take about 14.5g pressed powder C (pressed powder C consists of anhydrous slufuric acid zinc powder 5 weight part, Zinc oxide powder 0.5 weight part, dry coal ash 4.5 weight part), pour in beaker.
(3) measure 10ml with graduated cylinder and shift to an earlier date the good alkyd mixed solution of esterification.
(4) stir the pressed powder in beaker with glass stick, at leisure the alkyd mixed solution in graduated cylinder is poured into wherein, and constantly stir.Solid powder particle in beaker comparatively disperses but till being still in bond state.
(5) pressed powder absorbing alkyd mixed solution mixed thoroughly is encased in Boiling tube, and is ready in advance beyond the Great Wall and is inserted with the single hole soft rubber ball of conduit.Conveniently the mode of solid heating fixes device.
(6) with spirit lamp, to Boiling tube heating, (note preheating, whole mixt is heated evenly; The spirit lamp that moves around at leisure is needed in heat-processed), in time having gas to generate, as required, available drainage collects the gas of whole bottle; Also gas can be chewed by point and light; Or pass in the carbon tetrachloride solution of bromine or the acidic solution of potassium permanganate, carry out the relevant nature test of ethene.
The productive rate of the present embodiment ethene is 91.2%.When doing relevant nature with it, experimental phenomena is fairly obvious; When preparing glycol dibromide with it, effect is also fine.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (7)
1. the method for a Preparing Ethylene in Lab, it is characterized in that: 95% ethanol in experiment and the vitriol oil two kinds of liquid reagent pressed powders are all absorbed, experiment becomes solid reagent from liquid reagent, also changed into common Boiling tube by flask or distilling flask by the producer heated, and do not need thermometer is installed.
2. the method for Preparing Ethylene in Lab as claimed in claim 1, is characterized in that: the concrete steps of described method are as follows:
(1) 95% ethanol is mixed with the volume ratio of the vitriol oil by 1:3, make alkyd mixed solution, placed through 6-12 hour, make ethanol fully obtain esterification and generate vinic acid;
(2) take the pressed powder of mixing, pour in beaker, then measure the good alkyd mixed solution of esterification prepared by step (1) with graduated cylinder, also pour into wherein, then mix thoroughly, every 10-15g pressed powder adds 10ml alkyd mixed solution;
(3) the blended solid powder absorbing alkyd mixed solution mixed thoroughly is encased in Boiling tube, and the single hole soft rubber ball got ready in advance beyond the Great Wall, the mode of conveniently solid heating fixes device, can carry out producing and relevant property test of ethene.
3. the method for Preparing Ethylene in Lab as claimed in claim 1, is characterized in that: described pressed powder is the mixture of coal ash of anhydrous sulfate, metal oxide and drying, and its weight ratio is followed successively by 5-10 part; 0.1-1 part; 1-5 part.
4. the method for Preparing Ethylene in Lab as claimed in claim 3, is characterized in that: described pressed powder consist of anhydrous slufuric acid calcium powder 7 weight part, lime powder 0.5 weight part, dry coal ash 2.5 weight part.
5. the method for Preparing Ethylene in Lab as claimed in claim 3, is characterized in that: described pressed powder consist of anhydrous slufuric acid magnesium dust 6 weight part, magnesium oxide 0.35 weight part, dry coal ash 3.65 weight part.
6. the method for Preparing Ethylene in Lab as claimed in claim 3, is characterized in that: described anhydrous slufuric acid zinc powder 5 weight part, Zinc oxide powder 0.5 weight part, dry coal ash 4.5 weight part.
7. the method for Preparing Ethylene in Lab as claimed in claim 3, is characterized in that: described coal ash is the cinder ash from the drying of boiler house, obtains through 100 mesh sieve.
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| CN201510134325.3A CN104744198B (en) | 2015-03-25 | 2015-03-25 | A kind of method of Preparing Ethylene in Lab |
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| CN201510134325.3A CN104744198B (en) | 2015-03-25 | 2015-03-25 | A kind of method of Preparing Ethylene in Lab |
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| CN104744198B CN104744198B (en) | 2017-12-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268204A (en) * | 2016-09-18 | 2017-01-04 | 商洛学院 | Solid state concentrated sulphuric acid desiccant and preparation method thereof, application, renovation process |
| CN107488136A (en) * | 2017-09-04 | 2017-12-19 | 泰安汉威集团有限公司 | A kind of method for preparing ethero-sulfuric acid |
| CN113666798A (en) * | 2021-07-16 | 2021-11-19 | 上虞新和成生物化工有限公司 | Green process for preparing bromoethane from bromine salt |
| CN113666798B (en) * | 2021-07-16 | 2024-06-04 | 上虞新和成生物化工有限公司 | Green technology for preparing bromoethane from bromate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014001517A1 (en) * | 2012-06-29 | 2014-01-03 | Scientist Of Fortune S.A. | Process for producing a c2-c10 monoalkene employing a terpene synthase or a prenyl transferase |
-
2015
- 2015-03-25 CN CN201510134325.3A patent/CN104744198B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014001517A1 (en) * | 2012-06-29 | 2014-01-03 | Scientist Of Fortune S.A. | Process for producing a c2-c10 monoalkene employing a terpene synthase or a prenyl transferase |
Non-Patent Citations (3)
| Title |
|---|
| 刘立群: "加入生石灰制取乙烯气体的正交试验研究", 《化学教学》 * |
| 尹志刚: "实验室制备乙烯实验的研究和改进", 《科技信息（学术研究）》 * |
| 陈章福: "制乙烯气体时加生石灰的研究", 《化学教学》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268204A (en) * | 2016-09-18 | 2017-01-04 | 商洛学院 | Solid state concentrated sulphuric acid desiccant and preparation method thereof, application, renovation process |
| CN106268204B (en) * | 2016-09-18 | 2019-06-21 | 商洛学院 | Solid state concentrated sulfuric acid desiccant and preparation method thereof, application, regeneration method |
| CN107488136A (en) * | 2017-09-04 | 2017-12-19 | 泰安汉威集团有限公司 | A kind of method for preparing ethero-sulfuric acid |
| CN107488136B (en) * | 2017-09-04 | 2020-04-14 | 泰安汉威集团有限公司 | Method for preparing ethyl hydrogen sulfate |
| CN113666798A (en) * | 2021-07-16 | 2021-11-19 | 上虞新和成生物化工有限公司 | Green process for preparing bromoethane from bromine salt |
| CN113666798B (en) * | 2021-07-16 | 2024-06-04 | 上虞新和成生物化工有限公司 | Green technology for preparing bromoethane from bromate |
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