CN102229524A - Reaction device for synthesizing levo terpineol - Google Patents
Reaction device for synthesizing levo terpineol Download PDFInfo
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- CN102229524A CN102229524A CN2011100978330A CN201110097833A CN102229524A CN 102229524 A CN102229524 A CN 102229524A CN 2011100978330 A CN2011100978330 A CN 2011100978330A CN 201110097833 A CN201110097833 A CN 201110097833A CN 102229524 A CN102229524 A CN 102229524A
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Abstract
The invention provides a reaction device for synthesizing levo terpineol and relates to a reaction device with pipe type fixed bed reactors for synthesizing the levo terpineol. The reaction device mainly comprises an evaporation kettle, a condenser and 2 to 10 pipe type fixed bed reactors connected in parallel or in series. The reaction device pushes raw materials to circularly flow between the evaporation kettle and the pipe type fixed bed reactors through evaporation natural circulation, adopts evaporation and reaction separation to contribute to precisely controlling the contact time and the reaction temperature of the raw materials and a catalyst, improving selectivity of the reaction, reducing side reactions and increasing yield, is provided with an evaporation chamber and a demister on a heating kettle to contribute to separating the raw materials from the products, reducing the levo terpineol generated by the reaction and entrained to the pipe type fixed bed reactors and improving reaction efficiency, and adopts the pipe type fixed bed reactors to contribute to reducing abrasion of catalyst granules, avoiding inactivation and prolonging service life. The reaction device effectively solves the problems of low reaction selectivity, many side reactions and low yield in the conventional synthesized levo terpineol. By the reaction device, the synthetic reaction of the levo terpineol can be performed under the best process condition; and the yield can reach over 65 percent.
Description
Technical field
The present invention relates to a kind of chemical industry synthesizer, the reaction unit of especially synthetic L-terpineol.
Background technology
Terpineol 350 (terpineol) also claim Chinese parasol tree oil, terpinol, it is a kind of monocyclic monoterpene alcohol compound, have α-, β-, γ-three kind of isomer, wherein alpha-terpineol is the most common in nature, alpha-terpineol has left-handed, three kinds of optically active forms of dextrorotation and racemization, the commodity Terpineol 350 is a kind of racemic mixture based on alpha-terpineol, be colourless viscous liquid, has Syringa oblata Lindl. fragrance, it is one of main synthetic perfume kind, and has optically active left-handed alpha-terpineol, at desinsection, sterilization, aspects such as mosquito repellent show good effect, and its perviousness is strong, medicine is had certain synergism, at agricultural chemicals, medicine, aspects such as daily-use chemical industry have a extensive future.
At present, the industrial process of Terpineol 350 has two kinds: the one, and traditional sulfuric acid " two-step approach ", other method is " single stage method "." two-step approach " technology is complicated, long reaction time, and equipment is many, and energy consumption is big, and equipment corrosion is serious, and " three wastes " are seriously polluted, and poor selectivity, and side reaction is many, thereby the raw material consumption quota is high." single stage method " be turps in the presence of acid catalyst, directly carry out hydration one step to generate Terpineol 350.This method has advantages such as technical process is short, equipment is few, energy expenditure is low.Traditional Terpineol 350 reaction unit is the still formula substantially, have agitator, and the catalyzer of one-step synthesis L-terpineol is a solid acid catalyst, phenomenons such as granules of catalyst wearing and tearing, inactivation, life-span minimizing appear in tank reactor easily, reaction preference is relatively poor, by-product is more, has influenced the yield of Terpineol 350.Consider type of heating, thermal conductivity, the viscosity of raw material and the factors such as life-span of granules of catalyst of reactor, the reaction unit of one-step synthesis L-terpineol obviously is not suitable for selecting for use tank reactor.
Summary of the invention
The purpose of this invention is to provide a kind of feed stock conversion height, reaction unit is little, running cost is low, can prolong catalyst life, is suitable for the tubular fixed-bed reaction unit of the synthetic L-terpineol of scale operation.
The reaction unit of synthetic L-terpineol adopts tubular fixed-bed reactor, and device comprises evaporating kettle, condenser and tubular fixed-bed reactor group A, and described evaporating kettle bottom is a heating kettle, and the centre is an evaporator room, and evaporator room is provided with opening for feed; Scum dredger is arranged at the evaporating kettle top, and heating kettle is provided with chuck, can lead to the cooling of steam heating and cold water, and discharge port is arranged at the evaporating kettle bottom; Heating kettle, evaporator room connect into an integral body by flange bolt, the evaporating kettle top is connected with condenser by pipeline, condenser is by the tubular fixed-bed reactor group A of pipe connection below, and the outlet of tubular fixed-bed reactor group A inserts the evaporator room in the evaporating kettle.
Above-described tubular fixed-bed reactor group
Form by 2～10 tubular fixed-bed reactors, by pipeline and valve control, adopt parallel connection or placed in-line mode to be combined into an integral body between each tubular fixed-bed reactor; The tubular fixed-bed reactor group adopts the logical hot water heating of shell side, in be provided with catalyst loading tubulation and catalyzer supporting plate.
The outside surface of above-described evaporating kettle, tubular fixed-bed reactor is provided with thermal insulation layer, and the thermal insulation layer outer wall is a mortar, interior filling heat preservation rock.
Above-described condenser is provided with material is carried out refrigerative cold water or coolant system.
Above-described evaporating kettle, tubular fixed-bed reactor group A are equipped with temperature indicator and pressure display instrument table.
The part that above-described evaporating kettle, condenser, scum dredger, tubular fixed-bed reactor contact with material all adopts stainless material to make, and other parts are made of carbon steel material.
The part that above-described pipeline contacts with material all adopts stainless steel tube or Glass tubing, the other parts carbon steel pipe.
Catalyzer supporting plate in the above-described tubular fixed-bed reactor group A is a stainless steel porous card, adopts to flexibly connect the conveniently assemble and disassemble catalyzer.
Above-described tubular fixed-bed reactor is the tubular fixed-bed reactor of diameter 25～800mm, length 500～6000mm.
The tubular fixed-bed reaction unit of synthetic L-terpineol of the present invention, it is the reaction unit that a kind of industrialized one-step is produced L-terpineol, this device is by the evaporation natural circulation, promoting raw material circulates between evaporating kettle and tubular fixed-bed reactor, helping reaction product effectively separates with raw material, improve the selectivity of reaction, reduce side reaction, improve yield.
Advantage of this reaction unit and outstanding effect: by adopting evaporation and Reaction Separation, help accurately controlling the duration of contact and the temperature of reaction of raw material and catalyzer, improve the selectivity of reaction, reduce side reaction, improve yield; By evaporator room and scum dredger are set on heating kettle, help separating of raw material and product, reduce the L-terpineol that reaction generates and be entrained to the tubular fixed-bed reactor place, improve reaction efficiency; By adopting tubular fixed-bed reactor, help reducing the wearing and tearing of granules of catalyst, avoid inactivation, prolongs life.
The present invention can efficiently solve the problem that existing synthetic L-terpineol reaction preference is poor, side reaction is many, yield is low.The present invention can carry out the building-up reactions of L-terpineol under optimum process condition, yield reaches more than 65%.
Description of drawings
Fig. 1 is the structural representation of L-terpineol reaction unit of the present invention.
Embodiment
As shown in the figure, apparatus of the present invention mainly comprise evaporating kettle 4, condenser 5, tubular fixed-bed reactor group A.Evaporating kettle 4 includes heating kettle 1, evaporator room 2 and scum dredger 3, and heating kettle 1, evaporator room 2 connect into an integral body by flange bolt, and scum dredger 3 is contained in position, evaporator room 2 inner tip flange place.The part that evaporating kettle, condenser, tubular fixed-bed reactor contact with material all adopts stainless material to make, and other parts are made of carbon steel material; Scum dredger is made of stainless material.Tubular fixed-bed reactor group A is made up of 2～10 tubular fixed-bed reactors 6, by pipeline and valve control, adopts parallel connection or placed in-line mode to be combined into an integral body between each tubular fixed-bed reactor 6, is installed in condenser 5 belows.Be provided with catalyst loading tubulation 7, catalyzer supporting plate 8 in the tubular fixed-bed reactor 6, catalyzer supporting plate 8 is a stainless steel porous card, adopts to flexibly connect.Condenser 5 independently is installed in evaporating kettle 4 tops.Become a circulation loop by pipe connection between evaporating kettle 4, condenser 5 and the tubular fixed-bed reactor group A.The part that pipeline contacts with material all adopts stainless steel tube or Glass tubing, the other parts carbon steel pipe.Reaction unit also comprises corresponding temperature
Pressure
Display instrument.
Tubular fixed-bed reactor is the tubular fixed-bed reactor of diameter 25～800mm, length 500～6000mm.
Evaporating kettle adopts the logical steam heating of chuck and the logical cold water cooling of chuck, tubular fixed-bed reactor to adopt the logical hot water heating of shell side; Condenser is provided with material is carried out refrigerative cold water or coolant system.Described refrigerant can be the liquid higher than evaporation of water temperature, for example salt solution etc.
The outside surface of evaporating kettle, tubular fixed-bed reactor is provided with thermal insulation layer, and the thermal insulation layer outer wall is a mortar, interior filling heat preservation rock.
Operating process: various reaction raw materials are delivered in the heating kettle 1 by proportioning, close the charging valve, material heats in heating kettle 1, thermal source adopts steam, raw material and entrainer form the azeotrope evaporation and enter in the evaporator room 2, azeotrope and reaction product are disconnected from each other in evaporator room 2, the reaction product L-terpineol refluxes downwards, stay in the heating kettle 1, raw material then forms azeotropic steam and moves upward to enter in the condenser 5 and be condensed, scum dredger 3 can prevent that reaction product from being carried secretly upwards and flow, raw material enters after condensation among the tubular fixed-bed reactor group A and reacts, the reactor shell side feeds hot water and carries out temperature adjustment, tubular fixed-bed reactor group A is made up of 2～10 tubular fixed-bed reactors 6, variation according to reaction conditions is controlled by valve, adopt or and or the mode of string make up, raw material is back in the heating kettle 1 after reaction, the reaction product L-terpineol is stayed in the heating kettle 1, and unreacted raw material continuation flows among the tubular fixed-bed reactor group A with entrainer formation azeotropic steam cycle reacts; Behind 5～13 hours circulating reaction, steam off and hot water, heating kettle 1 feed cold water material are cooled off, and after finishing, material are emitted through discharge port.
Claims (9)
1. the reaction unit of a synthetic L-terpineol, it is characterized in that: this device adopts tubular fixed-bed reactor, equipment comprises evaporating kettle, condenser and tubular fixed-bed reactor group A, described evaporating kettle (4) bottom is heating kettle (1), the centre is evaporator room (2), and evaporator room (2) is provided with opening for feed; Scum dredger (3) is arranged at evaporating kettle (4) top, and heating kettle (1) is provided with chuck, can lead to the cooling of steam heating and cold water, and discharge port is arranged at heating kettle (1) bottom; Heating kettle (1), evaporator room (2) connect into an integral body by flange bolt, evaporating kettle (4) top is connected with condenser (5) by pipeline, condenser (5) is by the tubular fixed-bed reactor group A of pipe connection below, and the outlet of tubular fixed-bed reactor group A inserts the evaporator room (2) in the evaporating kettle.
2. the reaction unit of synthetic L-terpineol according to claim 1, it is characterized in that: tubular fixed-bed reactor group A is made up of 2～10 tubular fixed-bed reactors (6), by pipeline and valve control, adopt parallel connection or placed in-line mode to be combined into an integral body between each tubular fixed-bed reactor (6); Tubular fixed-bed reactor group A adopts the logical hot water heating of shell side, in be provided with catalyst loading tubulation (7) and catalyzer supporting plate (8).
3. according to the reaction unit of claim 1 and 2 described synthetic L-terpineols, it is characterized in that: the outside surface of described evaporating kettle (4), tubular fixed-bed reactor (6) is provided with thermal insulation layer, and the thermal insulation layer outer wall is a mortar, interior filling heat preservation rock.
4. the reaction unit of synthetic L-terpineol according to claim 1, it is characterized in that: condenser is provided with material is carried out refrigerative cold water or coolant system.
5. according to the reaction unit of claim 1 and 2 described synthetic L-terpineols, it is characterized in that: evaporating kettle, tubular fixed-bed reactor group are equipped with temperature indicator and pressure display instrument table.
6. according to the reaction unit of claim 1 and 2 described synthetic L-terpineols, it is characterized in that: the part that described evaporating kettle (4), condenser (5), scum dredger (3), tubular fixed-bed reactor (6) contact with material all adopts stainless material to make, and other parts are made of carbon steel material.
7. according to the reaction unit of claim 1 and 2 described synthetic L-terpineols, it is characterized in that: the part that described pipeline contacts with material all adopts stainless steel tube or Glass tubing, the other parts carbon steel pipe.
8. according to the reaction unit of claim 1 and 2 described synthetic L-terpineols, it is characterized in that: the catalyzer supporting plate (8) in the described tubular fixed-bed reactor group A is a stainless steel porous card, adopts to flexibly connect the conveniently assemble and disassemble catalyzer.
9. according to the reaction unit of claim 1 and 2 described synthetic L-terpineols, it is characterized in that: described tubular fixed-bed reactor (6) is the tubular fixed-bed reactor of diameter 25～800mm, length 500～6000mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100978330A CN102229524A (en) | 2011-04-19 | 2011-04-19 | Reaction device for synthesizing levo terpineol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100978330A CN102229524A (en) | 2011-04-19 | 2011-04-19 | Reaction device for synthesizing levo terpineol |
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| CN102229524A true CN102229524A (en) | 2011-11-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011100978330A Pending CN102229524A (en) | 2011-04-19 | 2011-04-19 | Reaction device for synthesizing levo terpineol |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976898A (en) * | 2012-12-21 | 2013-03-20 | 福建省清流县闽山化工有限公司 | Method for synthesizing terpilenol |
| CN106117121A (en) * | 2016-08-17 | 2016-11-16 | 南京红太阳生物化学有限责任公司 | A kind of device and method of synthesis 2,2 bipyridyls |
| CN109238413A (en) * | 2018-07-05 | 2019-01-18 | 河南中烟工业有限责任公司 | A method of improving low-temperature heat kettle static weighing the measuring precision |
| WO2020093749A1 (en) * | 2018-11-08 | 2020-05-14 | 广西化工研究院有限公司 | Fungicidal composition containing terpenol and chitosan and preparation method therefor and use thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197053A (en) * | 1998-05-06 | 1998-10-28 | 中国科学院广州化学研究所 | Method of directly preparing terpene hydrate alcohol by terpene |
| CN1482113A (en) * | 2003-07-16 | 2004-03-17 | 广西壮族自治区化工研究院 | Process for preparing levogyrate alpha-terpineol |
| CN201101899Y (en) * | 2007-09-10 | 2008-08-20 | 河南润恒生物能源有限公司 | Film evaporimeter |
-
2011
- 2011-04-19 CN CN2011100978330A patent/CN102229524A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197053A (en) * | 1998-05-06 | 1998-10-28 | 中国科学院广州化学研究所 | Method of directly preparing terpene hydrate alcohol by terpene |
| CN1482113A (en) * | 2003-07-16 | 2004-03-17 | 广西壮族自治区化工研究院 | Process for preparing levogyrate alpha-terpineol |
| CN201101899Y (en) * | 2007-09-10 | 2008-08-20 | 河南润恒生物能源有限公司 | Film evaporimeter |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976898A (en) * | 2012-12-21 | 2013-03-20 | 福建省清流县闽山化工有限公司 | Method for synthesizing terpilenol |
| CN102976898B (en) * | 2012-12-21 | 2015-06-10 | 福建省清流县闽山化工有限公司 | Method for synthesizing terpilenol |
| CN106117121A (en) * | 2016-08-17 | 2016-11-16 | 南京红太阳生物化学有限责任公司 | A kind of device and method of synthesis 2,2 bipyridyls |
| CN109238413A (en) * | 2018-07-05 | 2019-01-18 | 河南中烟工业有限责任公司 | A method of improving low-temperature heat kettle static weighing the measuring precision |
| WO2020093749A1 (en) * | 2018-11-08 | 2020-05-14 | 广西化工研究院有限公司 | Fungicidal composition containing terpenol and chitosan and preparation method therefor and use thereof |
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Application publication date: 20111102 |