CN103446948A - Reaction tower - Google Patents
Reaction tower Download PDFInfo
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- CN103446948A CN103446948A CN2013103780443A CN201310378044A CN103446948A CN 103446948 A CN103446948 A CN 103446948A CN 2013103780443 A CN2013103780443 A CN 2013103780443A CN 201310378044 A CN201310378044 A CN 201310378044A CN 103446948 A CN103446948 A CN 103446948A
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- reaction
- still
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- tower wall
- reaction chamber
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Abstract
The invention discloses a reaction tower which comprises a tower wall; a reaction cavity provided with a feeding hole is arranged in the tower wall; a heating pipe is arranged in the reaction cavity; the reaction cavity is internally provided with a temperature detection device extending outside the tower wall; the bottom of the reaction cavity is provided with a stirrer; the upper part of the reaction cavity in the tower wall is vertically provided with a fractional column; a fractional column temperature detection device is arranged at the section of the fractional column, extending outside the top of the tower wall; the fractional column is provided with a first still head and a second still head above the fractional column temperature detection device; the lower end of the first still head is connected with a distributor; the middle section of the first still head is provided with a condensation chamber provided with a condenser pipe; the distributor is provided with a discharge hole, a vacuumized air duct opening and a reflux port; the reflux port is connected with the second still head by a reflux pump. Compared with the prior art, the reaction tower improves the reaction conversion rate.
Description
Technical field
The present invention relates to chemical reaction equipment manufacturing technology field, especially a kind of consersion unit for the reaction of alkene class terpenoid.
Background technology
The reaction tower of existing alkene class terpenoid reaction, generally to be provided with the reaction chamber with charging aperture and discharging opening in the tower wall, be provided with heating tube in reaction chamber, be provided with temperature-detecting device in reaction chamber, with the detection reaction temperature, this temperature-detecting device reaches outside reaction chamber, and the reaction chamber bottom of some reaction tower is provided with agitator.In the course of reaction of some alkene class terpenoids; especially in the course of reaction of using the synthetic 4-acetyl group of 3-carene and the direct acidylate of acetic anhydride-2-carene, because its conversion ratio is always lower, reaction speed is always slower; cause processing cost higher, be not suitable for batch production.Through repetition test for many years; the factors such as reaction pressure and temperature are made to continuous change; analyze its reason; when in finding to react, the product acetic acid of 3-carene mixture and acetic anhydride increases; the speed of separating out of acetic acid is slack-off; thereby slow down whole reaction speed, finally reach a molecular balance, affect 4-acetyl group-2-carene yield simultaneously.Therefore need a kind of reaction tower of design; to change the reaction speed of the intermediate product in course of reaction; for example the speed of separating out of the product acetic acid of 3-carene mixture and acetic anhydride in the course of reaction of 4-acetyl group-2-carene, speed to reach the purpose that reaction speed improves reaction conversion ratio simultaneously.
Summary of the invention
The invention provides a kind of reaction tower, can change the intermediate product speed of separating out in course of reaction, increase reaction conversion ratio.
In order to address the above problem, technical scheme of the present invention is: this reaction tower includes the tower wall, be provided with the reaction chamber with charging aperture in described tower wall, be provided with heating tube in described reaction chamber, be provided with in described reaction chamber and stretch out the outer temperature-detecting device of described tower wall, described reaction chamber bottom is provided with agitator, reaction chamber top in described tower wall vertically is provided with still, the section that this still stretches out described Ta Bi top is provided with the still temperature-detecting device, described still is provided with the first fractional still head and after-fractionating head in described still temperature-detecting device top, the lower end of described the first fractional still head is connected with distributor, the interlude of described the first fractional still head is provided with the condensation chamber with condenser pipe, described distributor is provided with discharge gate, the air channel opening and the refluxing opening that vacuumize, this refluxing opening connects described after-fractionating head by reflux pump.
Owing to having adopted technique scheme, the present invention compared with prior art has following beneficial effect:
This reaction tower, adopt the top of reaction tower that Packed still is set, still by filler distills out reaction intermediate at tower top, and by controlling different vacuum conditioned reaction temperature, and reflux and recently control the discharging speed of intermediate product acetic acid by adjusting, the positive reaction power of organic reaction is strengthened, to improve the conversion ratio of reaction.
The accompanying drawing explanation
Fig. 1 is the structural representation of the embodiment of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail:
Reaction tower as shown in Figure 1, it includes tower wall 1, be provided with the reaction chamber 5 with charging aperture 4 in tower wall 1, be provided with heating tube 3 in reaction chamber 5, be provided with in reaction chamber 5 and stretch out the outer temperature-detecting device 2 of tower wall 1, reaction chamber 5 bottoms are provided with agitator 17, reaction chamber 5 tops in tower wall 1 vertically are provided with still 6, the section that this still 6 stretches out tower wall 1 top is provided with temperature-detecting device 2, and still 6 is provided with the first fractional still head 8 and after-fractionating 7 in temperature-detecting device 2 tops; The condensation chamber 9 lower than the first fractional still head 8 positions that the first fractional still head 8 connects with condenser pipe 10, the bottom of condensation chamber 9 is provided with outlet, the outlet of condensation chamber 9 connects the charging aperture 15 of distributor 13, air channel opening 14 and refluxing opening 12 that distributor 13 is provided with discharge gate 16, vacuumizes, this refluxing opening 12 connects after-fractionatings 7 by reflux pump 11; Air channel opening 14 can connect vacuum buffer tank and vavuum pump.Use this reaction tower; 3-carene mixture and acetic anhydride are processed into 4-acetyl group-2-carene; logical capillary bubbling vacuumizes heating; vacuum degree control is at-0.09MPa; the tower interior reaction temperature is at 80 ° of C～85 ° C; the tower top of reaction tower starts to separate out acetic acid; the still 6 of reaction chamber 5 top fillers; separate out acetic acid speed by the backflow fractionation of adjusting 6 two minutes two of still in 3～5 Grams Per Hour scopes than controlling; within 8 hours, start reactant is carried out to sample analysis; until 3-carene content stops heating after being less than 3%, be cooled to below 40 ℃, stop the vacuum discharging.Being washed to neutrality analyzes: 3-carene content is: 2.6%, 4-acetyl group-2-carene content is: 78.82%, and conversion ratio is 97%, is selectively: 85%.
Claims (1)
1. a reaction tower, include the tower wall, be provided with the reaction chamber with charging aperture in described tower wall, be provided with heating tube in described reaction chamber, be provided with in described reaction chamber and stretch out the outer temperature-detecting device of described tower wall, described reaction chamber bottom is provided with agitator, it is characterized in that: the reaction chamber top in described tower wall vertically is provided with still, the section that this still stretches out described Ta Bi top is provided with the still temperature-detecting device, described still is provided with the first fractional still head and after-fractionating head in described still temperature-detecting device top, the lower end of described the first fractional still head is connected with distributor, the interlude of described the first fractional still head is provided with the condensation chamber with condenser pipe, described distributor is provided with discharge gate, the air channel opening and the refluxing opening that vacuumize, this refluxing opening connects described after-fractionating head by reflux pump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103780443A CN103446948A (en) | 2013-08-27 | 2013-08-27 | Reaction tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103780443A CN103446948A (en) | 2013-08-27 | 2013-08-27 | Reaction tower |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103446948A true CN103446948A (en) | 2013-12-18 |
Family
ID=49730029
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013103780443A Pending CN103446948A (en) | 2013-08-27 | 2013-08-27 | Reaction tower |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103446948A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111231A (en) * | 1994-05-03 | 1995-11-08 | 中国石油化工总公司上海石油化工研究院 | Process for synthesis of dimethyl ether by catalytic distillation |
| CN101932543A (en) * | 2007-11-30 | 2010-12-29 | 巴斯夫欧洲公司 | Method for producing optically active, racemic menthol |
| CN202893344U (en) * | 2012-09-11 | 2013-04-24 | 南通大学 | Continuously and frequently stirring kettle-type external circulating reaction rectification device with built-in horizontal type coil pipe |
| CN103215066A (en) * | 2012-12-12 | 2013-07-24 | 滁州市润达溶剂有限公司 | Distillation separation device and method for liquid hydrocarbon mixture |
-
2013
- 2013-08-27 CN CN2013103780443A patent/CN103446948A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1111231A (en) * | 1994-05-03 | 1995-11-08 | 中国石油化工总公司上海石油化工研究院 | Process for synthesis of dimethyl ether by catalytic distillation |
| CN101932543A (en) * | 2007-11-30 | 2010-12-29 | 巴斯夫欧洲公司 | Method for producing optically active, racemic menthol |
| CN202893344U (en) * | 2012-09-11 | 2013-04-24 | 南通大学 | Continuously and frequently stirring kettle-type external circulating reaction rectification device with built-in horizontal type coil pipe |
| CN103215066A (en) * | 2012-12-12 | 2013-07-24 | 滁州市润达溶剂有限公司 | Distillation separation device and method for liquid hydrocarbon mixture |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131218 |