CN102584630A - Method for synthesizing methacrylic acid isocyanate ethyl ester - Google Patents
Method for synthesizing methacrylic acid isocyanate ethyl ester Download PDFInfo
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- CN102584630A CN102584630A CN2011104384238A CN201110438423A CN102584630A CN 102584630 A CN102584630 A CN 102584630A CN 2011104384238 A CN2011104384238 A CN 2011104384238A CN 201110438423 A CN201110438423 A CN 201110438423A CN 102584630 A CN102584630 A CN 102584630A
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- ethyl acetate
- methacrylic acid
- methylacrylic acid
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Abstract
A method for synthesizing methacrylic acid isocyanate ethyl ester is characterized in that ethyl acetate is used as a solvent and is mixed with methacrylic acid-ethanolamine hydrochloride, then the methacrylic acid-ethanolamine hydrochloride, a stabilizing agent and a catalyst are dissolved into the ethyl acetate according to a certain proportion, quantitative trichloromethyl carbonic ester ethyl acetate solution is dripped at different temperatures, then rectification and separation are carried out, a target product is obtained in a reaction kettle by the reaction in three steps, namely raw material preparation, synthesis and separation, and the total recovery is more than or equal to 75%. The method for synthesizing the methacrylic acid isocyanate ethyl ester has the positive effects that the problems of high safety risk, resulting from the monitoring of the formation reaction with the participation of highly toxic chemicals (phosgene), are avoided.
Description
Technical field
The invention belongs to technical field of chemistry, relate to a kind of compound method of methylacrylic acid isocyanato ethyl ester.
Technical background
General formula does
The methylacrylic acid isocyanic acid close ethyl ester.
This title product is the sticking agent of superior performance, and outstanding anti-aging and insulating property are arranged, and cohesive strength is high, is mainly used in high-end electronic product.
Its related methods of synthesis structure splits, and synthesis step is many, long flow path, yield are low, needs to use the hypertoxic chemical of monitoring (phosgene) to feed and participates in reaction, generation title product in the main raw material.(phosgene is a kind of strong stimulation, choke damp, sucks phosgene and can cause wet lung, and pneumonia etc. have the danger of causing death), security risk is high.
Summary of the invention
In order to overcome above-mentioned technical deficiency, the invention provides a kind of method of synthesize methyl acrylic acid isocyanato ethyl, need monitor hypertoxic chemical (phosgene) participation formation reaction, problems such as security risk height to solve prior art.
Technical solution technical scheme that problem adopts of the present invention:
Make solvent with ETHYLE ACETATE; Mix with methylacrylic acid-ethanolamine hydrochloric salt; Be dissolved in methylacrylic acid-ethanolamine hydrochloric salt, stablizer, catalyzer in the ETHYLE ACETATE by a certain percentage; Under the different temperature section, drip quantitative trichloromethyl carbonate ethyl acetate solution through rectifying separation, branch differing temps section is accomplished three-step reaction and is got title product, total recovery in a reaction kettle: >=75%
The compound method step of title product:
One, raw material is equipped with: stablizer, catalyzer, methylacrylic acid-ethanolamine hydrochloric salt are dissolved in ethyl acetate solvent by the proportioning of 1:3～6:200～300; The trichloromethyl carbonate ethyl acetate solution 400～500L of preparation 20～40%.
Two, building-up process: temperature is under 40-50 ℃ of situation; The proportioning that the equal speed of trichloromethyl carbonate ethyl acetate solution 300～400L with 20～40% splashes into stablizer, catalyzer, methylacrylic acid-ethanolamine hydrochloric salt 1:3～6:200～300 is dissolved in in the ethyl acetate solvent; Be warmed up to backflow after dripping off; And keeping 20-30 hour reflux state to drip the trichloromethyl carbonate ethyl acetate solution down, middle control is to terminal.
Three, separate: place stage number 30 towers to get title product content (GL) reaction solution: >=99% through rectifying separation.Rectifying gained solvent recuperation is applied mechanically.
Methylacrylic acid: ethanolamine hydrochloride (mole) 1.0～1.5:1.0.
Adopting positively effect of the present invention is to have avoided participating in formation reaction, problems such as security risk height because of monitoring hypertoxic chemical (phosgene).
Description of drawings
Accompanying drawing 1 is a process flow sheet of the present invention.
Embodiment
One, raw material is equipped with: stablizer, catalyzer, methylacrylic acid-ethanolamine hydrochloric salt are dissolved in ethyl acetate solvent by the proportioning of 1:3.5:220; The trichloromethyl carbonate ethyl acetate solution 450L of preparation 35%.
Two, synthetic: temperature is under 42-44 ℃ of situation; The proportioning that the equal speed of trichloromethyl carbonate ethyl acetate solution 350L with 35% splashes into stablizer, catalyzer, methylacrylic acid-ethanolamine hydrochloric salt 1:3～6:200～300 is dissolved in in the ethyl acetate solvent; Be warmed up to backflow after dripping off; And keeping 26-30 hour reflux state to drip remaining 100L trichloromethyl carbonate ethyl acetate solution down, middle control is to terminal.
Three, separate: place stage number 30 towers to get title product content (GL) reaction solution: >=99% through rectifying separation.Rectifying gained solvent recuperation is applied mechanically.
Methylacrylic acid: ethanolamine hydrochloride (mole) 1.2:1.0.
Claims (1)
1. the method for synthesize methyl acrylic acid isocyanato ethyl; It is characterized in that making solvent with ETHYLE ACETATE; Mix with methylacrylic acid-ethanolamine hydrochloric salt, methylacrylic acid-ethanolamine hydrochloric salt, stablizer, catalyzer are dissolved in the ETHYLE ACETATE by a certain percentage, under the different temperature section, drip quantitative trichloromethyl carbonate ethyl acetate solution through rectifying separation; Branch differing temps section is accomplished three-step reaction and is got title product, total recovery in a reaction kettle: >=75%; The synthesis step of its title product is following:
(1) raw material is equipped with: stablizer, catalyzer, methylacrylic acid-ethanolamine hydrochloric salt are dissolved in ethyl acetate solvent by the proportioning of 1:3～6:200～300; The trichloromethyl carbonate ethyl acetate solution 400～500L of preparation 20～40%;
(2) synthetic: temperature is under 40-50 ℃ of situation; The proportioning that the equal speed of trichloromethyl carbonate ethyl acetate solution 300～400L with 20～40% splashes into stablizer, catalyzer, methylacrylic acid-ethanolamine hydrochloric salt 1:3～6:200～300 is dissolved in in the ethyl acetate solvent; Be warmed up to backflow after dripping off; And keeping 20-30 hour reflux state to drip the trichloromethyl carbonate ethyl acetate solution down, middle control is to terminal;
(3) separate: place stage number 30 towers to get title product content (GL) reaction solution through rectifying separation: >=99%, rectifying gained solvent recuperation is applied mechanically; Methylacrylic acid: ethanolamine hydrochloride (mole) 1.0～1.5:1.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104384238A CN102584630A (en) | 2011-12-24 | 2011-12-24 | Method for synthesizing methacrylic acid isocyanate ethyl ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104384238A CN102584630A (en) | 2011-12-24 | 2011-12-24 | Method for synthesizing methacrylic acid isocyanate ethyl ester |
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| Publication Number | Publication Date |
|---|---|
| CN102584630A true CN102584630A (en) | 2012-07-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011104384238A Pending CN102584630A (en) | 2011-12-24 | 2011-12-24 | Method for synthesizing methacrylic acid isocyanate ethyl ester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113261A (en) * | 2013-01-21 | 2013-05-22 | 张家港瀚康化工有限公司 | Preparation method of metharcylic acid, 2-isocyanatoethyl ester |
| CN103193675A (en) * | 2013-03-26 | 2013-07-10 | 浙江同丰医药化工有限公司 | Method for preparing ethyl methacrylate isocyanate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6452746A (en) * | 1987-08-25 | 1989-02-28 | Showa Rhodia Chem | Production of unsaturated carboxylic acid isocyanatoalkyl ester |
| CN1475479A (en) * | 2002-08-13 | 2004-02-18 | 浙江工业大学 | Chemical synthesis method of isopropyl isocyanate |
| CN1478769A (en) * | 2003-05-08 | 2004-03-03 | 蔡戈冬 | Chemical synthesis method of 3,4-dichlorobenzene isocyanate |
| CN1939899A (en) * | 2005-09-26 | 2007-04-04 | 杭州崇舜化学有限公司 | Synthesis of 1,5-naphthalene isocyanate |
-
2011
- 2011-12-24 CN CN2011104384238A patent/CN102584630A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6452746A (en) * | 1987-08-25 | 1989-02-28 | Showa Rhodia Chem | Production of unsaturated carboxylic acid isocyanatoalkyl ester |
| CN1475479A (en) * | 2002-08-13 | 2004-02-18 | 浙江工业大学 | Chemical synthesis method of isopropyl isocyanate |
| CN1478769A (en) * | 2003-05-08 | 2004-03-03 | 蔡戈冬 | Chemical synthesis method of 3,4-dichlorobenzene isocyanate |
| CN1939899A (en) * | 2005-09-26 | 2007-04-04 | 杭州崇舜化学有限公司 | Synthesis of 1,5-naphthalene isocyanate |
Non-Patent Citations (6)
| Title |
|---|
| 《化学试剂》 20020630 韩莹等 "异氰酸酯的简单合成法" 第375页, 第1-2段 1 第24卷, 第6期 * |
| 《化工中间体》 20020731 洪新民 "固体光气的合成与应用" 第16页, (4) 1 , 第7期 * |
| 《应用化工》 20080930 王向辉等 "三光气法合成取代苯异氰酸酯" 全文 1 第37卷, 第9期 * |
| 洪新民: ""固体光气的合成与应用"", 《化工中间体》 * |
| 王向辉等: ""三光气法合成取代苯异氰酸酯"", 《应用化工》 * |
| 韩莹等: ""异氰酸酯的简单合成法"", 《化学试剂》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113261A (en) * | 2013-01-21 | 2013-05-22 | 张家港瀚康化工有限公司 | Preparation method of metharcylic acid, 2-isocyanatoethyl ester |
| CN103193675A (en) * | 2013-03-26 | 2013-07-10 | 浙江同丰医药化工有限公司 | Method for preparing ethyl methacrylate isocyanate |
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Application publication date: 20120718 |