CN102211987A - Method for preparing 3-cyclohexene-1-formaldehyde - Google Patents
Method for preparing 3-cyclohexene-1-formaldehyde Download PDFInfo
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- CN102211987A CN102211987A CN2010105654649A CN201010565464A CN102211987A CN 102211987 A CN102211987 A CN 102211987A CN 2010105654649 A CN2010105654649 A CN 2010105654649A CN 201010565464 A CN201010565464 A CN 201010565464A CN 102211987 A CN102211987 A CN 102211987A
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- formaldehyde
- tetrahydrobenzene
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- purity
- cyclohexene
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Abstract
The invention relates to a method for preparing 3-cyclohexene-1-formaldehyde by using butadiene and acrolein as raw materials. The method for preparing the 3-cyclohexene-1-formaldehyde comprises the following steps of: polymerizing the butadiene and the acrolein serving as raw materials to obtain a gas-liquid mixture of the 3-cyclohexene-1-formaldehyde, wherein the purity of the butadiene raw material is more than or equal to 99.3 percent, the purity of the acrolein is more than or equal to 98 percent, the polymerization temperature is 240 to 300 DEG C and the reaction pressure is 10 to 20MPa; and obtaining the 3-cyclohexene-1-formaldehyde product by separating. The preparation method is simple in process; the reclamation rate reaches 70 percent; the preparation method is easy in operation and high in reaction speed; the product is stable and reliable in quality; and the preparation method is environment-friendly, and can be industrially implemented.
Description
Technical field
The present invention relates to a kind of is the method that raw material has been produced 3-tetrahydrobenzene-1-formaldehyde with divinyl and propenal.
Background technology
3-tetrahydrobenzene-1-formaldehyde is a kind of important Organic Chemicals, is widely used in the production of medicine, food, agrochemicals, feed, polyester and other fine chemical products.For example: 3-tetrahydrobenzene-1-formaldehyde and CO and H2 reaction generate hydroxymethyl-cyclohexane, and hydroxymethyl-cyclohexane and phthalic acid condensation can be made synthon etc.
Many now employing divinyl and propenal are that raw material has been produced 3-tetrahydrobenzene-1-formaldehyde.In the production process, technology is wayward, and polyreaction is slow, and the rate of recovery is low, and end product quality is difficult to reach requirement.
Summary of the invention
Purpose of the present invention is exactly that proposing a kind of is the method that raw material has been produced 3-tetrahydrobenzene-1-formaldehyde with divinyl and propenal in order to address the above problem.
Technical scheme provided by the invention is:
A kind of method of producing 3-tetrahydrobenzene-1-formaldehyde, with divinyl, propenal is raw material, obtain the liquid-vapor mixture of 3-tetrahydrobenzene-1-formaldehyde by polymerization, used raw material divinyl purity is 〉=99.3%, the purity of propenal is 〉=98%, described polymerization temperature 240-300 ℃, reaction pressure is 10-20Mpa, and then obtains 3-tetrahydrobenzene-1-formaldehyde products through separating.
Concrete, the molar ratio of propenal, divinyl is between 1.4～2.0 ︰ 1.
Concrete, described polymerization reaction time is 12～18 hours, transformation efficiency is 80%, selectivity 90%.
Concrete, heat thermal oil that described polyreaction produces or fused-salt medium are derived.
Concrete, described polymeric reaction product distills, and tower top temperature is 110-120 ℃, and the tower top pressure table is at 0.05-0.1Mpa, reflux ratio 6-10.
Concrete, cat head obtains 3-tetrahydrobenzene-1-formaldehyde products, and purity is 〉=98%.
Preparation method technology of the present invention is simple, and the rate of recovery is up to 70%, and is easy to operate, and speed of response is fast, stable and reliable product quality, environmentally safe, but industrializing implementation.
Embodiment
A kind of method of producing 3-tetrahydrobenzene-1-formaldehyde, with divinyl, propenal is raw material, obtain the liquid-vapor mixture of 3-tetrahydrobenzene-1-formaldehyde by polymerization, used raw material divinyl purity is 〉=99.3%, and the purity of propenal is 〉=98%, described polymerization temperature is controlled at 270 ℃, reaction pressure is 16Mpa, and the molar ratio of propenal, divinyl is at 1.7 ︰ 1, and polymerization reaction time is 15 hours, transformation efficiency is 80%, selectivity 90%.Described polymeric reaction product distills, and tower top temperature is 115 ℃, and the tower top pressure table is at 0.08Mpa, reflux ratio 8.
The heat that described polyreaction produces is derived with thermal oil or fused-salt medium.
After testing, cat head obtains 3-tetrahydrobenzene-1-formaldehyde products, and purity is 〉=98%.
Should be noted that at last: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the field are to be understood that: still can make amendment or the part technical characterictic is equal to replacement the specific embodiment of the present invention; And not breaking away from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope that the present invention asks for protection.
Claims (6)
1. method of producing 3-tetrahydrobenzene-1-formaldehyde, with divinyl, propenal is raw material, it is characterized in that: the liquid-vapor mixture that obtains 3-tetrahydrobenzene-1-formaldehyde by polymerization, used raw material divinyl purity is 〉=99.3%, the purity of propenal is 〉=98%, described polymerization temperature 240-300 ℃, reaction pressure is 10-20Mpa, and then obtains 3-tetrahydrobenzene-1-formaldehyde products through separating.
2. according to claim 1 described a kind of method of producing 3-tetrahydrobenzene-1-formaldehyde, it is characterized in that: the molar ratio of propenal, divinyl is between 1.4～2.0 ︰ 1.
3. according to claim 1 described a kind of method of producing 3-tetrahydrobenzene-1-formaldehyde, it is characterized in that: described polymerization reaction time is 12～18 hours, and transformation efficiency is 80%, selectivity 90%.
4. according to claim 1 described a kind of method of producing 3-tetrahydrobenzene-1-formaldehyde, it is characterized in that: the heat that described polyreaction produces is derived with thermal oil or fused-salt medium.
5. according to the described a kind of method of producing 3-tetrahydrobenzene-1-formaldehyde of claim 1 to 3 any claim, it is characterized in that: described polymeric reaction product distills, tower top temperature is 110-120 ℃, and the tower top pressure table is at 0.05-0.1Mpa, reflux ratio 6-10.
6. according to claim 5 described a kind of methods of producing 3-tetrahydrobenzene-1-formaldehyde, it is characterized in that: cat head obtains 3-tetrahydrobenzene-1-formaldehyde products, and purity is 〉=98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105654649A CN102211987A (en) | 2010-11-30 | 2010-11-30 | Method for preparing 3-cyclohexene-1-formaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105654649A CN102211987A (en) | 2010-11-30 | 2010-11-30 | Method for preparing 3-cyclohexene-1-formaldehyde |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102211987A true CN102211987A (en) | 2011-10-12 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105654649A Pending CN102211987A (en) | 2010-11-30 | 2010-11-30 | Method for preparing 3-cyclohexene-1-formaldehyde |
Country Status (1)
| Country | Link |
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| CN (1) | CN102211987A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4642387A (en) * | 1985-01-19 | 1987-02-10 | Degussa Aktiengesellschaft | Process for the production of 3-cyclohexene-1-carboxaldehyde |
| CN101239864A (en) * | 2007-08-29 | 2008-08-13 | 武汉新景化工有限责任公司 | Method and device for synthesizing six-membered cyclic compound by continuous method |
-
2010
- 2010-11-30 CN CN2010105654649A patent/CN102211987A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4642387A (en) * | 1985-01-19 | 1987-02-10 | Degussa Aktiengesellschaft | Process for the production of 3-cyclohexene-1-carboxaldehyde |
| CN101239864A (en) * | 2007-08-29 | 2008-08-13 | 武汉新景化工有限责任公司 | Method and device for synthesizing six-membered cyclic compound by continuous method |
Non-Patent Citations (1)
| Title |
|---|
| 于浩等: "脂环族环氧化物的合成与应用(三)环己烯酯环氧树脂", 《热固性树脂》 * |
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Application publication date: 20111012 |