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CN111056975A - Method for removing acetone from acetonitrile product - Google Patents

Method for removing acetone from acetonitrile product Download PDF

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Publication number
CN111056975A
CN111056975A CN201911203010.4A CN201911203010A CN111056975A CN 111056975 A CN111056975 A CN 111056975A CN 201911203010 A CN201911203010 A CN 201911203010A CN 111056975 A CN111056975 A CN 111056975A
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CN
China
Prior art keywords
acetonitrile
acetone
dinitrophenylhydrazine
solution
removing acetone
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.)
Pending
Application number
CN201911203010.4A
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Chinese (zh)
Inventor
庆九
俞新南
朱小刚
刘芳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nantong Liyang Chemical Co ltd
NANTONG ACETIC ACID CHEMICAL CO Ltd
Original Assignee
Nantong Liyang Chemical Co ltd
NANTONG ACETIC ACID CHEMICAL CO Ltd
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Publication date
Application filed by Nantong Liyang Chemical Co ltd, NANTONG ACETIC ACID CHEMICAL CO Ltd filed Critical Nantong Liyang Chemical Co ltd
Priority to CN201911203010.4A priority Critical patent/CN111056975A/en
Publication of CN111056975A publication Critical patent/CN111056975A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00Preparation of carboxylic acid nitriles
    • C07C253/32Separation; Purification; Stabilisation; Use of additives
    • C07C253/34Separation; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of chemical industry, and particularly relates to a method for removing acetone from acetonitrile, which comprises the following steps: (1) the method comprises the steps of taking 98-99% acetonitrile as a raw material, taking about 40-50ppm acetone and 1-8% mass concentration 2, 4-dinitrophenylhydrazine solution, weighing a certain amount of 2, 4-dinitrophenylhydrazine and acetonitrile according to the molar ratio of the acetone to the 2, 4-dinitrophenylhydrazine of 1:1-1:2, mixing, stirring, heating and starting reflux. (2) Controlling the reflux time for 10min-2h to remove all acetone in the obtained acetonitrile product. The process can completely remove trace acetone in the acetonitrile. The process is simple to operate, is suitable for industrial amplification and has practical value.

Description

Method for removing acetone from acetonitrile product
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for removing acetone from acetonitrile products.
Background
Acetonitrile, english name: acetonitrile, alias: methyl cyanide, molecular formula and molecular weight: C2H3N ═ 41.05; physical and chemical properties: appearance: colorless liquid with pungent odor; melting Point (. degree. C.): -45.7; boiling point (. degree.C., atmospheric pressure): 81-82; flash point (. degree. C.): 6; solubility: is miscible with water and soluble in most organic solvents such as alcohol.
Acetonitrile is a solvent with wide application and excellent performance, and can be mixed and dissolved with water, various inorganic substances and organic substances. Can be used as solvent for synthetic fiber, or used as solvent for extracting fat from animal and vegetable oil in oil industry, or used as excellent reaction solvent, and has special dissolution property and phase transferability, and is favorable for improving reaction yield. The carbon-nitrogen triple bond of acetonitrile is easy to generate nitrile addition reaction, can be used in the field of fine chemical industry, and is an important intermediate for the synthetic reaction of medicines and pesticides. The pure acetonitrile can be used as an organic modifier and a solvent of thin-layer chromatography, paper chromatography, spectrum, liquid chromatography and polarography, in particular to be used as a mobile phase of high performance liquid chromatography, and the analysis precision can reach more than ppb level.
The prior art introduces a method for removing impurities such as hydrocyanic acid, acrylonitrile and the like in ① acetonitrile, the method comprises the steps of adding a strong oxidant for reaction, rectifying and filtering to obtain high-purity acetonitrile, the method for removing water in ② acetonitrile comprises the steps of mixing the water-containing acetonitrile with alkali, separating acetonitrile and a water phase, removing the water phase, distilling the obtained acetonitrile to obtain purified acetonitrile, passing the obtained purified acetonitrile through cation exchange resin to obtain the high-purity acetonitrile, ③ adding a strong acid strong base salt and a hydrocarbon solvent into the waste acetonitrile, oscillating, standing, layering, adding potassium permanganate peroxide, heating, distilling, and finally introducing an adsorbent filled with activated carbon for adsorption to obtain the high-purity acetonitrile.
The documents and patents that employ the above methods are as follows:
1. a method for preparing full brilliant, yellow straight and plum blossom red plum, a mass spectrum level acetonitrile and a device thereof,
[P].CN:102432498A.2011-10-28
2. high-purity acetonitrile
[P].CN:101171233A.2008-4-30
3. Purification method of high-purity organic solvent acetonitrile from Shanghai Shaoxing high-purity solvent Co
[P].CN:201310753989.9.2015-7-1
These documents and patents employ different methods for removing impurities from acetonitrile, but none of the prior art provides a method for removing acetone from acetonitrile.
Disclosure of Invention
The invention aims to provide a method for effectively removing acetone from acetonitrile, which comprises the steps of taking acetonitrile as a raw material, weighing a 2, 4-dinitrophenylhydrazine solution into the acetonitrile according to a molar ratio, starting stirring and heating, and simultaneously carrying out reflux, wherein the obtained acetonitrile product does not contain acetone impurities. The method can completely remove acetone, does not influence the acetonitrile content, has simple process, is suitable for industrial amplification and has great practical value.
The invention adopts the following technical scheme:
a method for removing acetone from acetonitrile products comprises the following steps:
(1) weighing 2, 4-dinitrophenylhydrazine and acetonitrile, and mixing, wherein the acetonitrile contains an organic component of 98-99% and contains 40-50ppm of acetone; the 2, 4-dinitrophenylhydrazine is a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 1% -8%, the materials are fed according to the molar ratio of acetone to 2, 4-dinitrophenylhydrazine of 1:1-1:2, stirred and heated, and the reflux is started;
(2) controlling the reflux time for 10min-2h, and completely removing the acetone in the obtained acetonitrile product.
Further, the reflux time in the step (2) is controlled to be 30 min-60 min.
Further, the 2, 4-dinitrophenylhydrazine solution is acetonitrile solution of 2, 4-dinitrophenylhydrazine.
Further, the rotation speed of the stirring in the step (1) is 100-300 rpm/min.
Further, the heating rate in the step (1) is 5-10 ℃/h.
Further, the mass concentration range of the 2, 4-dinitrophenylhydrazine is 2-6%.
Further, the molar ratio of the acetone to the 2, 4-dinitrophenylhydrazine is 1:1 to 1.15.
Further, the reflux time is 10min-60 min.
In the method for removing acetone from acetonitrile, acetonitrile is firstly added into a reaction kettle, a 2, 4-dinitrophenylhydrazine solution is added according to a proportion, electric stirring is started, the stirring speed is set to be 100-300rpm/min, electric heating of the reaction kettle is started, the temperature rise speed is set to be 5-10 ℃, the solution starts to flow back, the reflux time is controlled to be 10min-2h, and all the acetone in the obtained acetonitrile is removed.
The acetonitrile contains 98-99% of acetonitrile organic components, and contains 40-50ppm of acetone, wherein the acetone is a byproduct in acetonitrile production.
In the invention, acetone and 2, 4-dinitrophenylhydrazine are used for reacting to generate 2, 4-dinitrophenylhydrazone, so that the boiling point difference between the acetone and acetonitrile is improved, and the acetone can be separated by distillation subsequently.
The invention has the beneficial effects that:
the process can completely remove trace acetone in the acetonitrile; the process is simple to operate, is suitable for industrial amplification and has practical value.
Detailed Description
The following provides a specific example of the method for removing acetone from acetonitrile product.
Comparative example 1: a method for removing acetone from acetonitrile products comprises the following steps:
acetonitrile with the content of organic components of 98-99 percent is used as a raw material, acetone is 45ppm, and a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 1 percent is prepared at room temperature, wherein the weight ratio of acetone: weighing a certain amount of 2, 4-dinitrophenylhydrazine solution into acetonitrile, starting stirring and heating, opening cooling water of a return pipe for refluxing, and controlling heating to keep the solution refluxing for 1h, wherein the acetone content is 20 ppm.
Example 2: a method for removing acetone from acetonitrile products comprises the following steps:
acetonitrile with the content of organic components of 98-99 percent is used as a raw material, 40ppm of acetone is used for preparing a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 4 percent at room temperature, and the reaction is carried out according to the molar ratio of acetone: weighing a certain amount of 2, 4-dinitrophenylhydrazine solution into acetonitrile, starting stirring and heating, opening cooling water of a return pipe for refluxing, controlling heating to keep the solution for refluxing for 30min, and detecting no acetone in the product.
Example 3: a method for removing acetone from acetonitrile products comprises the following steps:
acetonitrile with the content of organic components of 98-99 percent is used as a raw material, acetone is 45ppm, and a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 6 percent is prepared at room temperature, wherein the weight ratio of acetone: weighing a certain amount of 2, 4-dinitrophenylhydrazine solution into acetonitrile, starting stirring and heating, opening cooling water of a return pipe for refluxing, controlling heating to keep the solution for refluxing for 45min, and detecting no acetone in the product.
Example 4: a method for removing acetone from acetonitrile products comprises the following steps:
acetonitrile with the content of organic components of 98-99 percent is used as a raw material, 50ppm of acetone is used for preparing a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 4 percent at room temperature, and the reaction is carried out according to the molar ratio of acetone: weighing a certain amount of 2, 4-dinitrophenylhydrazine solution into acetonitrile, starting stirring and heating, opening cooling water of a return pipe for refluxing, controlling heating to keep the solution for refluxing for 60min, and detecting no acetone in the product.
Example 5A method for removing acetone from the product acetonitrile:
acetonitrile with the content of organic components of 98-99 percent is used as a raw material, acetone is 48ppm, and a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 4 percent is prepared at room temperature, wherein the weight ratio of acetone: weighing a certain amount of 2, 4-dinitrophenylhydrazine solution into acetonitrile, starting stirring and heating, opening cooling water of a return pipe for refluxing, controlling heating to keep the solution for refluxing for 45min, and detecting no acetone in the product.
Example 6: industrial scale-up
Putting 3000L (initial acetone 40-50ppm) of acetonitrile which is a raw material and has the organic component content of 98-99% into a 5000L stirring reaction kettle, starting stirring, and adding acetone: adding 10L of 2, 4-dinitrophenylhydrazine solution with the mass concentration of 5% at room temperature, starting heating, opening a cooling water reflux pipe to reflux, controlling the heating to keep the solution to reflux for 0.5h, and detecting no acetone in the product.
The invention analyzes the content of acetone in acetonitrile by gas chromatography, and the detection conditions are as follows: the FID detector and capillary column are adopted, the temperature is raised to 200 ℃ at the speed of 10 ℃/min, the temperature is kept for 20min, N2 is used as carrier gas, and the sample injection amount is 0.2-0.4 mu L.
The present invention has been disclosed in terms of the preferred embodiment, but it is not intended to be limited to the embodiment, and all technical solutions obtained by substituting or converting the equivalent embodiments fall within the scope of the present invention.

Claims (8)

1. A method for removing acetone from acetonitrile products is characterized by comprising the following steps:
(1) weighing 2, 4-dinitrophenylhydrazine and acetonitrile, and mixing, wherein the acetonitrile contains an organic component of 98-99% and contains 40-50ppm of acetone; the 2, 4-dinitrophenylhydrazine is a 2, 4-dinitrophenylhydrazine solution with the mass concentration of 1% -8%, the materials are fed according to the molar ratio of acetone to 2, 4-dinitrophenylhydrazine of 1:1-1:2, stirred and heated, and the reflux is started;
(2) controlling the reflux time for 10min-2h, and completely removing the acetone in the obtained acetonitrile product.
2. The method for removing acetone from acetonitrile as a product according to claim 1, wherein the reflux time in the step (2) is controlled to be 30-60 min.
3. The method for removing acetone from acetonitrile as a product according to claim 1, wherein the solution of 2, 4-dinitrophenylhydrazine is a solution of 2, 4-dinitrophenylhydrazine in acetonitrile.
4. The method for removing acetone from acetonitrile as claimed in claim 1, wherein the stirring speed in step (1) is 100-300 rpm/min.
5. The method for removing acetone from acetonitrile as a product according to claim 1, wherein the heating rate in step (1) is 5-10 ℃/h.
6. The method for removing acetone from acetonitrile as a product according to claim 1, wherein the mass concentration of the 2, 4-dinitrophenylhydrazine is within a range of 2-6%.
7. The method for removing acetone from acetonitrile as a product according to claim 1, wherein the molar ratio of acetone to 2, 4-dinitrophenylhydrazine is 1: 1-1.15.
8. The method for removing acetone from acetonitrile as a product according to claim 1, wherein the refluxing time is 10min to 60 min.
CN201911203010.4A 2019-11-29 2019-11-29 Method for removing acetone from acetonitrile product Pending CN111056975A (en)

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CN111056975A true CN111056975A (en) 2020-04-24

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1231282A (en) * 1998-02-23 1999-10-13 标准石油公司 Improved purification and recovery of acetonitrile
CN102895837A (en) * 2012-02-13 2013-01-30 中国人民解放军海军医学研究所 Composition used for eliminating compounds of aldehydes and ketones
CN103163270A (en) * 2013-03-28 2013-06-19 中国烟草总公司郑州烟草研究院 Method for detecting eight volatile carbonyl compounds in cigarette filter tip through liquid chromatography-tandem mass spectrometry
CN107935887A (en) * 2017-12-21 2018-04-20 上海应用技术大学 A kind of preparation method of gradient level acetonitrile
CN109476619A (en) * 2016-07-20 2019-03-15 巴斯夫欧洲公司 Method for purifying propylene oxide

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1231282A (en) * 1998-02-23 1999-10-13 标准石油公司 Improved purification and recovery of acetonitrile
CN102895837A (en) * 2012-02-13 2013-01-30 中国人民解放军海军医学研究所 Composition used for eliminating compounds of aldehydes and ketones
CN103163270A (en) * 2013-03-28 2013-06-19 中国烟草总公司郑州烟草研究院 Method for detecting eight volatile carbonyl compounds in cigarette filter tip through liquid chromatography-tandem mass spectrometry
CN109476619A (en) * 2016-07-20 2019-03-15 巴斯夫欧洲公司 Method for purifying propylene oxide
CN107935887A (en) * 2017-12-21 2018-04-20 上海应用技术大学 A kind of preparation method of gradient level acetonitrile

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Application publication date: 20200424