CN104262153A - Technology method capable of continuously carrying out methyl acetoacetate production - Google Patents
Technology method capable of continuously carrying out methyl acetoacetate production Download PDFInfo
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- CN104262153A CN104262153A CN201410428637.0A CN201410428637A CN104262153A CN 104262153 A CN104262153 A CN 104262153A CN 201410428637 A CN201410428637 A CN 201410428637A CN 104262153 A CN104262153 A CN 104262153A
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- tower
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- methyl acetoacetate
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- thermal insulation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/46—Preparation of carboxylic acid esters from ketenes or polyketenes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a technology method capable of continuously carrying out methyl acetoacetate production, and relates to the technology field of chemical raw material production. The technology production comprises the following steps: adding a methyl acetate finished product into an esterification reactor as a reactor substrate, simultaneously dropwise adding DK and methanol into the reactor; cooling the sleeve of the esterification reactor; keeping on dropwise adding until the fluid in the esterification reactor starts to overflow to the thermal insulation reactor; adding diketene from the overflow pipe; when the fluid in the thermal insulation reactor reaches a certain amount, making the methyl acetoacetate in the thermal insulation reactor overflow to the thermal insulation transfer tank at a constant temperature; pumping the coarse methyl acetoacetate in the thermal insulation transfer tank to a rectifying tower; feeding the coarse product into the rectifying tower from the middle of the rectifying tower, increasing the vacuum degree, carrying out rectification under a certain reflux state so as to obtain finished products; and discharging light components from the tower top, finished products from the middle of the tower, and slag from the tower bottom. The provided technology method is capable of improving work efficiency, greatly increasing the production power, reducing part of steam energy consumption, and saving the equipment investment, can carry out rectification in one tower, and thus reduces the steam energy consumption, moreover the operation is easy to control, and products with a high content are more easily obtained.
Description
Technical field:
The present invention relates to the production technical field of industrial chemicals, be specifically related to one and carry out methyl acetoacetate producing and manufacturing technique continuously.
Background technology:
Methyl acetoacetate is a kind of important organic synthesis intermediate, and it is of many uses, and its derivative is mostly the kind that tonnage is larger, answers focus development pesticide intermediate, medicine intermediate at present, to meet the need of market.
Methyl acetoacetate effect is extensive, and in pesticide industry, methyl acetoacetate is mainly used in synthetic pesticide diazinon, propylene weeding chrysanthemum in pesticide industry, weedicide pyrazolate, benzofenap, pyrazoxyfen, sterilant hymexazol etc.Chemical assistant, methyl acetoacetate except as except cellulose ester solvent, can also to synthesize as antimalarial agent, the solvent of spices, coating; In addition as solvent synthesis aluminium alcoholates and sequestrant, for the thickening of resin modified, printing-ink, improve bounding force etc.; Can also as polymerizing catalyst, for the preparation of the metal complex etc. with aluminium, chromium etc.; Pharmaceutical industries, methyl acetoacetate pharmaceutical industries main for the synthesis of cephalo element class antibiotic important intermediate to hydroxyglycine Deng Shi salt, in addition can also the raw material METHYL 3 AMINO CROTONATE etc. of synthetic vessel expander dipyridamole and antiepileptic drug intermediate valproic acid and calcium antagonist; VITAMIN, the Application Areas that methyl acetoacetate most is dived is for the synthesis of serial VITAMIN, the raw material phantol that what current consumption was maximum is for the synthesis of vitamin-E and different vegetable alcohol; Methyl acetoacetate can synthesize β-ionone, and these product are the important source material preparing vitamin A and carotene; Methyl acetoacetate can also synthesize vitamin B13, and also known as vitamin B13, vitamin B13 as the medicine for the treatment of hepatic diseases, and can participate in the synthesis of nucleic acid, has very much development potentiality as healthcare products etc.; Methyl acetoacetate can the raw material α ethanoyl-gamma-butyrolactone of synthesise vitamins B1; Organic synthesis, methyl acetoacetate can synthesize multiple important fine-chemical intermediate, wherein it should be noted that most methyl ethyl diketone and 2,6-picoline; Dye industry, methyl acetoacetate can synthesize the dyestuff intermediate of the important aniline series of various new as raw material, in addition all right synthesizing pyrazole quinoline ketone intermediate, and these products are promising new dye, Pigment Intermediates.
In China, the production of methyl acetoacetate and acyl acid ethyl acetate is also carried out in many factories on same production equipment.According to incompletely statistics, domestic production total capacity reaches 10,000 t/a, and actual output reaches 5000t/a.Actual year consumption about 10,000 t of current China, therefore domestic some produce medicine, commodity that the every average annual import of unit of agricultural chemicals is certain satisfy the demand, year import volume be about 5000t, market value is 1.3 ten thousand-1.5 ten thousand yuan/t.The content of China's product is in the past about 97.0% in addition, can not meet market demand.Along with China's medicine industry develop rapidly, the especially exploitation of vitamin medicaments and calcium antagonist medicine, in the urgent need to high-quality product, namely product content is greater than 99.0%, but current production technique can not reach such requirement.
Summary of the invention:
The object of this invention is to provide one and carry out methyl acetoacetate producing and manufacturing technique continuously, its process design science, increase work efficiency, production capacity improves greatly, cooling is not needed after reaction terminates, directly enter in rectifying tower and heat up, reduce part steam-energy consumption, save facility investment, rectifying in a tower, reduce the energy consumption of steam, operation is easy to control, the product of the high-content that is more easy to get.
In order to solve the problem existing for background technology, the present invention is by the following technical solutions: its production technique is: in esterifying kettle, 1, put into ethyl ester methyl acetate finished product as still bed material, in still, drip DK and methyl alcohol simultaneously; 2, esterifying kettle chuck cooling; 3, when esterifying kettle be added drop-wise to a certain amount of after, start to insulation still in overflow; 4, ketene dimer is added from upflow tube; 5, when insulation still reach a certain amount of after, insulation still in the insulation limit overflow of methyl acetoacetate limit to insulation transfer tank; 6, by insulation transfer tank pump, thick ethyl ester methyl acetate is squeezed into rectifying tower; 7, rectifying tower charging from tower, gas clean-up, under certain reflux state, rectifying draws finished product; 8, rectifying tower ejects chieftain, and tower middle and upper part goes out Cheng Kou, arranges residue at the bottom of tower.
Principle of the present invention is:
Material reaction is thrown in by segmentation between original by esterification workshop section, changes continuous esterification into.Increase work efficiency, production capacity improves greatly, does not need cooling, directly enter in rectifying tower and heat up after reaction terminates, and reduces part steam-energy consumption.
Rectification section, by the original high and low Liang Taota that boils, changes a set of tower into and goes out high and low thing and the finished product of boiling simultaneously.Save facility investment, rectifying in a tower, reduce the energy consumption of steam, operation is easy to control, the product of the high-content that is more easy to get.
Embodiment:
This embodiment is by the following technical solutions: its production technique is: in esterifying kettle, 1, put into ethyl ester methyl acetate finished product as still bed material, in still, drip DK and methyl alcohol simultaneously; 2, esterifying kettle chuck cooling; 3, when esterifying kettle be added drop-wise to a certain amount of after, start to insulation still in overflow; 4, ketene dimer is added from upflow tube; 5, when insulation still reach a certain amount of after, insulation still in the insulation limit overflow of methyl acetoacetate limit to insulation transfer tank; 6, by insulation transfer tank pump, thick ethyl ester methyl acetate is squeezed into rectifying tower; 7, rectifying tower charging from tower, gas clean-up, under certain reflux state, rectifying draws finished product; 8, rectifying tower ejects chieftain, and tower middle and upper part goes out Cheng Kou, arranges residue at the bottom of tower.
Material reaction is thrown in by segmentation between original by the esterification workshop section of this embodiment, changes continuous esterification into.Increase work efficiency, production capacity improves greatly, does not need cooling, directly enter in rectifying tower and heat up after reaction terminates, and reduces part steam-energy consumption; Rectification section, by the original high and low Liang Taota that boils, changes a set of tower into and goes out high and low thing and the finished product of boiling simultaneously.Save facility investment, rectifying in a tower, reduce the energy consumption of steam, operation is easy to control, the product of the high-content that is more easy to get.
Claims (1)
1. carry out methyl acetoacetate producing and manufacturing technique continuously, it is characterized in that its production technique is: (1), in esterifying kettle, put into ethyl ester methyl acetate finished product as still bed material, in still, drip DK and methyl alcohol simultaneously; (2), esterifying kettle chuck cooling; (3), when esterifying kettle be added drop-wise to a certain amount of after, start to insulation still in overflow; (4), ketene dimer is added from upflow tube; (5), when insulation still reach a certain amount of after, insulation still in the insulation limit overflow of methyl acetoacetate limit to insulation transfer tank; (6), by insulation transfer tank pump, thick ethyl ester methyl acetate is squeezed into rectifying tower; (7), rectifying tower charging from tower, gas clean-up, under certain reflux state, rectifying draws finished product; (8), rectifying tower ejects chieftain, and tower middle and upper part goes out Cheng Kou, arranges residue at the bottom of tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410428637.0A CN104262153A (en) | 2014-08-27 | 2014-08-27 | Technology method capable of continuously carrying out methyl acetoacetate production |
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| CN201410428637.0A CN104262153A (en) | 2014-08-27 | 2014-08-27 | Technology method capable of continuously carrying out methyl acetoacetate production |
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| CN104262153A true CN104262153A (en) | 2015-01-07 |
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| CN201410428637.0A Pending CN104262153A (en) | 2014-08-27 | 2014-08-27 | Technology method capable of continuously carrying out methyl acetoacetate production |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384631A (en) * | 2015-11-24 | 2016-03-09 | 江苏天成生化制品有限公司 | Process of continuously producing methyl acetoacetate |
| CN107986962A (en) * | 2017-12-14 | 2018-05-04 | 山东汇海医药化工有限公司 | A kind of method that acetoacetic ester is recycled in the bottoms from acetoacetic ester |
| CN111825553A (en) * | 2019-04-17 | 2020-10-27 | 青岛海湾精细化工有限公司 | Preparation method of methyl acetoacetate |
Citations (5)
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|---|---|---|---|---|
| CN1280122A (en) * | 1999-07-08 | 2001-01-17 | 南通醋酸化工厂 | Method for producing acetylacetic ester |
| CN1483719A (en) * | 2002-08-09 | 2004-03-24 | 大赛璐化学工业株式会社 | Wethod for preparation acetylacetic ester |
| CN101029006A (en) * | 2007-04-13 | 2007-09-05 | 中国科学院山西煤炭化学研究所 | Method for synthesizing methyl acetoacetate methyl-carbonate and acetone |
| CN102101829A (en) * | 2009-12-22 | 2011-06-22 | 上海吴泾化工有限公司 | Process for preparing acetoacetic ester |
| CN202116468U (en) * | 2011-06-09 | 2012-01-18 | 江苏天成生化制品有限公司 | Device for producing methyl acetoacetate continuously |
-
2014
- 2014-08-27 CN CN201410428637.0A patent/CN104262153A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280122A (en) * | 1999-07-08 | 2001-01-17 | 南通醋酸化工厂 | Method for producing acetylacetic ester |
| CN1483719A (en) * | 2002-08-09 | 2004-03-24 | 大赛璐化学工业株式会社 | Wethod for preparation acetylacetic ester |
| CN101029006A (en) * | 2007-04-13 | 2007-09-05 | 中国科学院山西煤炭化学研究所 | Method for synthesizing methyl acetoacetate methyl-carbonate and acetone |
| CN102101829A (en) * | 2009-12-22 | 2011-06-22 | 上海吴泾化工有限公司 | Process for preparing acetoacetic ester |
| CN202116468U (en) * | 2011-06-09 | 2012-01-18 | 江苏天成生化制品有限公司 | Device for producing methyl acetoacetate continuously |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384631A (en) * | 2015-11-24 | 2016-03-09 | 江苏天成生化制品有限公司 | Process of continuously producing methyl acetoacetate |
| CN107986962A (en) * | 2017-12-14 | 2018-05-04 | 山东汇海医药化工有限公司 | A kind of method that acetoacetic ester is recycled in the bottoms from acetoacetic ester |
| CN111825553A (en) * | 2019-04-17 | 2020-10-27 | 青岛海湾精细化工有限公司 | Preparation method of methyl acetoacetate |
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Application publication date: 20150107 |