CN103285613A - Infinite reflux reaction distillation device of synthesizing terpineol and synthesizing method of device - Google Patents
Infinite reflux reaction distillation device of synthesizing terpineol and synthesizing method of device Download PDFInfo
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Abstract
The invention discloses an infinite reflux reaction distillation device of synthesizing terpineol and a synthesizing method of the device, and relates to terpineol. The device is provided with an evaporator, an evaporation tower, a condensing coil, a catalyst material basket and a heating jacket. The synthesizing method comprises the following steps of: placing the condensing coil in the catalyst material basket, mixing and filling a catalyst and a theta-ring stainless steel screen padding in the catalyst material basket, fixing the mixture in the evaporation tower and sealing; closing an emptying valve, adding a raw material into the evaporator, and closing a feeding valve; heating the evaporator to ensure that the raw material and a solvent are evaporated and condensed in the catalyst material basket, and carrying out catalytic reaction after condensed liquid contacts the catalyst; ensuring that a reaction product and the unreacted raw material in the catalyst material basket flow back to the evaporator at the bottom of the tower by virtue of gravity and terpilenol is left in the evaporator, condensing in the catalyst material basket and reacting again; stopping heating when the content of pinene subjected to sampling analysis from the evaporator is less than 10%, stopping reaction, and opening the emptying valve to discharge material for rectification saparation, thus obtaining the terpineol.
Description
Technical field
The present invention relates to terpinol, especially relate to a kind of total reflux reaction distilling apparatus and synthetic method thereof of synthetic terpinol.
Background technology
Terpinol is a kind of important chemical product, is widely used in industry such as essence and flavoring agent, medicine, plastics, soap and telecommunication.The prior synthesizing method of terpinol is two step method ([1] Chen Xiaopeng, Zhang Yunming. the research [J] of terpini hydras catalytic dehydration terpinol processed. the Guangxi chemical industry, 1992,21 (3): 4-6), be that turpentine oil (main component is firpene) is under fluid sulphuric acid catalysis, obtain terpini hydras through the hydration of open loop isomery, dewater then terpinol, but this technology have the production cycle long, energy consumption is high, equipment corrosion and shortcoming such as seriously polluted.Some scholars have carried out research widely to the catalyst of one-step method direct hydration terpinol processed at present, attempt with organic acid catalyst, molecular sieve catalyst ([3] Takakom, Ryuichiroo, Naotoh, et al.Hydration of pinene over hydrophobic zeolites in1,4-dioxane water and in water[J] .Microporous and Mesoporous Materials, 2007,101 (1/2): 176-183), solid super acid catalyst ([4] Chen Shaofeng, Guo Haifu, Yan Peng, etc. solid super-strong acid Ni/SO
4 2--SnO
2The hydration of catalysis firpene prepares terpinol [J]. chemistry world, 2009 (7): 430-435), cation exchange resin catalyst, ionic-liquid catalyst and film catalyst etc. replace the fluid sulphuric acid catalyst.In one-step technology, turpentine oil direct hydration under the acidic catalyst effect generates terpinol, that this technology has is with short production cycle, do not have advantages such as equipment corrosion and basic non-pollutant discharge substantially, but the optimization research and development of technical process are not enough, have that feed stock conversion is not high, product terpinol yield is lower, side reaction is more and the process energy consumption than problems such as height.
In recent years, the researcher has carried out the research exploration to reaction process and the synthetic method thereof of the synthetic terpinol of one-step method both at home and abroad, the catalyst that adopts mainly contains solid acid and liquid acid, and reaction process mainly contains technical process such as stirred-tank reactor catalysis method, injection-type reactor catalysis method and fixed bed reactors catalysis method.([2] Roman Aguirre M such as Roman, De la Torre Saenz L, Wilber Antunez Flore, et al.Synthesis of terpineol from a-pinene by homogeneous acid catalysis[J] .Catalysis Today, 2005,107-108:310-314) utilize stirred-tank reactor, having studied with liquid acid hydrochloric acid, monoxone, oxalic acid and acetic acid respectively is the synthetic terpinol of catalyst one-step method, the result shows that chloroacetic catalytic effect is best.When temperature is 70 ℃, water, firpene and chloroacetic mol ratio are 1: 2.4: 1.68 o'clock, and the conversion ratio of australene is 100%, and the yield of terpinol is 69.6%.But this method is catalyst with the liquid organic acid, still has the follow-up separation process complexity, problem such as equipment corrosion, " three wastes " are seriously polluted.([5] Yang Gaodong, Liu Yong, Shao Yuyin such as Yang Gaodong, Zhou Zheng, Zhang Zhi is bright. turpentine oil direct hydration repercussion study [J]. and Chemical Engineering, 2010,18(12): 48-52) utilize the pilot-scale injection-type reactor, make catalyst with cationic ion-exchange resin, reaction time is 4h, and research obtains terebinthine conversion ratio and is about 85%, and the yield of terpinol is about 35%, but the terpinol yield is lower, and the process energy consumption is higher.Wei Yi, Huang Kelin etc. ([6] Chinese patent CN102229524A) utilize a cover fixed-bed catalytic reactor, be that catalyst carries out the synthetic of terpinol with the resin, but have still that the product back-mixing is serious, the catalytic reaction time is long, problem such as side reaction easily takes place.And domestic and international synthetic reaction of the more employing stirred-tank reactor of the research of one-step method being carried out terpinol, the method generally needs organic acid as auxiliary agent, and need a large amount of solvents so that raw material fully mixes to promote reaction, therefore still there is the follow-up separation process complexity, problem such as equipment corrosion, " three wastes " are seriously polluted, the more important thing is that these class methods cause the damage of breaking of solid catalyst easily, seriously reduced life of catalyst, so cost increase greatly.Though and fixed bed reactors have solved the life of catalyst problem, but still exist product terpinol and catalyst long time of contact in the technical process, accessory substance composition and content are higher, the terpinol yield is hanged down and reached energy consumption than problems such as height, and its technology is further improved.
Summary of the invention
The objective of the invention is to prepare the problem that the terpinol technical process exists at existing one-step catalytic turpentine oil, a kind of total reflux reaction distilling apparatus and synthetic method thereof of synthetic terpinol is provided.
The total reflux reaction distilling apparatus of described synthetic terpinol is provided with evaporimeter, evaporating column, condenser coil, catalyst material basket, heating jacket; Described evaporimeter is provided with high steam entrance, feed(raw material)inlet, hot water outlet, temperature sensor and control interface, pressure sensor and remote alarm interface and discharging opening; Described evaporimeter top is connected with evaporating column, catalyst material basket is located in the evaporating column, and condenser coil is located in the catalyst material basket and with catalyst and is contacted, and described evaporating column outside is provided with heating jacket and heat-insulation layer, the bottom of evaporating column is provided with hot water inlet, and the top of evaporating column is provided with hot water outlet; The condenser coil two ends are cooling water inlet and coolant outlet.
Can be provided with the charging valve on the described feed(raw material)inlet; Can be provided with dispensing valve on the described discharging opening.
The method of described synthetic terpinol adopts the total reflux reaction distilling apparatus that synthesizes terpinol, and step is as follows:
1) condenser coil is put into catalyst material basket, again catalyst and θ ring stainless steel cloth filler mixed packing are gone in the catalyst material basket, and catalyst material basket is fixed in the evaporating column closed evaporating tower;
2) close dispensing valve, raw pine fuel-economizing, water and solvent are joined in the evaporimeter by the charging valve, close the charging valve;
3) evaporimeter is heated, make the evaporation of raw material and solvent and condensation in catalyst material basket, the condensate liquid contact catalyst carries out catalytic reaction; Because the evaporating column outer wall has heating jacket and heat-insulation layer, so only condensation in catalyst material basket of steam; The mixed liquor of raw material and solvent forms azeotropic in the evaporation process; Product in the catalyst material basket and unreacted raw material rely on gravity reflux at the bottom of the tower in the evaporimeter, and terpinol is deposited in the evaporimeter, and raw material and solvent evaporate azeotropic again, and condensation in catalyst material basket, react again; When the content of sample analysis firpene from evaporimeter＜10%, stop the heating of evaporimeter, cessation reaction, open the dispensing valve of base of evaporator, discharges material is carried out rectifying again and is separated, material obtains the terpinol product by the rectifying separation, and the unreacted raw material of rectifying gained and solvent are reused in the Returning evaporimeter again.
In step 1), described catalyst can adopt cationic ion-exchange resin, and it is the cationic ion-exchange resin of each model such as Amberlyst15, Amberlyst35, Amberlyst36 that described cationic ion-exchange resin can be selected model for use; Voidage in the described catalyst material basket can be 25%～35%; The loadings of described catalyst can be 7%～10% of raw material gross mass by mass percentage;
In step 2) in, described solvent can adopt the low-carbon (LC) alcohols, and the mass ratio of described turpentine oil, water, solvent can be 5: (1.5～2): (3～3.5).
In step 3), the purpose that described evaporating column outside is provided with heating jacket and heat-insulation layer is to avoid steam in the condensation of tower wall; Described condenser coil places catalyst material basket, by the flow of condensed water in the adjustment condenser coil and condensation and the reaction temperature in the temperature control catalyst material basket; Described catalytic reaction is in 6h, and the mass concentration of firpene can be less than 10% in the evaporimeter, and described product is separated through rectifying again, and unreacted raw material and solvent return the total reflux reaction distilling apparatus again and reuse; Mainly contain minor by-products such as citrene, terpinolene, amphene in the described product, namely can obtain the terpinol product by distillation operation.
The technical solution used in the present invention is to be raw material with turpentine oil (main component is firpene) and water, make solvent with low-carbon (LC) alcohols or ester class (ethyl acetate), make catalyst with large hole cation exchanger resin, under the proportioning of certain raw material and solvent, utilize the principle of reactive distillation, in the total reflux reaction distilling apparatus of design voluntarily, carry out catalyzing and synthesizing of terpinol, obtain higher firpene conversion ratio and terpinol yield, catalyst is continuously nearly 100 times in the reaction experiment, and catalytic performance is constant substantially.Product and accessory substance mainly are: alpha-terpineol, β-terpinol, γ-terpinol, 4-terpinol, D-citrene, terpinolene etc.
The as a whole apparatus for reactive distillation of total reflux reaction distilling apparatus of synthetic terpinol of the present invention, evaporimeter top is communicated with evaporating column, and catalyst material basket places evaporating column inside, and condenser coil places catalyst material basket fully to contact with catalyst.Raw material and solvent evaporate in evaporimeter, because the evaporating column outside is provided with heating jacket and heat-insulation layer, so steam only contacts cold catalyst material basket and is condensed in evaporating column, condensate liquid (comprises water, firpene, solvent) catalyst in the contact material basket reacts, the terpinol that reaction generates and unreacted raw material and solvent flow out the material basket fast and break away from catalyst, rely on gravity all to be back at the bottom of the tower in the evaporimeter, lower boiling water wherein, firpene and solvent continue evaporation, condensation, reaction and the cyclic process that refluxes, the then enrichment in evaporimeter of high boiling product terpinol.When the terpinol in the analyzing and testing evaporimeter or firpene concentration reach certain index, whole materials to be discharged by evaporimeter carry out rectifying and separate, the unreacted raw material of rectifying gained and solvent can return this device and reuse.
Outstanding advantage of the present invention:
(1) among the present invention, do not use any organic acid as reaction promoter, the solvent of use is pollution-free, do not have corrosion, and easily separates recyclable recycling with product.
(2) among the present invention, all technical process are carried out in a W-response distillation equipment, finish evaporation, the condensation of raw material, the full step cycle of reaction continuously automatically.Raw material and solvent form azeotropic vaporization in evaporimeter, the only condensation and reacting in catalyst material basket of rising steam.The product terpinol flows out the disengaging catalyst rapidly from the outer pit canal of material basket, and dependence gravity all is back at the bottom of the tower in the evaporimeter, thereby avoids the Long contact time catalyst and side reaction takes place.In addition, be back to the boiling point of terpinol of evaporimeter far above the azeotropic point of raw material and solvent, participate in reaction so terpinol can not evaporate contact catalyst again, thereby avoid the generation of side reaction, effectively control accessory substance and generate.
(3) among the present invention, catalyst material basket is suspended in the evaporating column, and evaporimeter places the evaporating column bottom, the unreacted feed liquid that refluxes downwards from catalyst material basket contacts with solvent vapo(u)r with the high temperature raw material of rising, part is vaporized to rise and enters catalyst material basket, and condensation is reacted again, thereby has shortened the circulating path of reaction raw materials and solvent, reduced the heating load of evaporimeter, made whole process realize lower energy consumption.The estimation result shows that energy consumption is lower than conventional two-step method more than 25%, and energy-saving effect is obvious.
Description of drawings
Fig. 1 forms schematic diagram for the structure of the total reflux reaction distilling apparatus embodiment of synthetic terpinol.
Fig. 2 is the GC-MS spectrogram of product.
The specific embodiment
Referring to Fig. 1, the total reflux reaction distilling apparatus embodiment of synthetic terpinol of the present invention is provided with evaporimeter A, evaporating column B, condenser coil C, catalyst material basket D, heating jacket E; Described evaporimeter A is provided with high steam entrance A1, feed(raw material)inlet A2, hot water outlet A3, temperature sensor and control interface A4, pressure sensor and remote alarm interface A5 and discharging port A 6; Described evaporimeter A top is connected with evaporating column B, catalyst material basket D is located in the evaporating column B, condenser coil C is located among the catalyst material basket D and with catalyst and contacts, described evaporating column B outside is provided with heating jacket E and heat-insulation layer (not drawing) in Fig. 1, the bottom of evaporating column B is provided with hot water inlet B1, and the top of evaporating column B is provided with hot water outlet B2; Condenser coil C two ends are cooling water inlet C1 and coolant outlet C2.Can be provided with charging valve V1 on the described feed(raw material)inlet A2; Can be provided with dispensing valve V2 on the described discharging port A 6.
TEMP and control system T comprise: cooling, temperature demonstration and temperature control (using the normal temperature cooling water control), the heating of evaporating column B outer wall chuck and the temperature of the heating of reaction raw materials among the evaporimeter A, temperature demonstration and temperature control (with providing steam for oneself or directly adding thermal control), condenser coil C show (generally only needing the temperature demonstration).
The total reflux reaction distil process process of the synthetic terpinol of catalyzing turpentine oil of the present invention is: at first, condenser coil C is put into catalyst material basket D, again catalyst and θ ring stainless steel cloth filler mixed packing are gone among the catalyst material basket D, and catalyst material basket D is fixed in the evaporating column B closed evaporating tower B; Secondly, close dispensing valve V
2, with turpentine oil, water and solvent according to certain proportioning by charging valve V
1Add among the evaporimeter A, close charging valve V
1A heats to evaporimeter, makes the evaporation of raw material and solvent and condensation in catalyst material basket D, and the condensate liquid contact catalyst carries out catalytic reaction.Because evaporating column B outer wall has heating jacket E and heat-insulation layer, so only condensation in catalyst material basket D of steam.The mixed liquor of raw material and solvent forms azeotropic in the evaporation process, and its temperature remains unchanged substantially.The temperature of condensate liquid and condensing liquid quantity flow and the temperature control by regulating cooling water in the condenser coil among the catalyst material basket D; Carrying out along with reaction, product among the catalyst material basket D and unreacted raw material rely on gravity to be back to fast at the bottom of the tower among the evaporimeter A, because the boiling point of product terpinol is far above the azeotropic point of raw material and solvent, therefore terpinol is deposited among the evaporimeter A, and raw material and solvent evaporate azeotropic again, and condensation in catalyst material basket D, react again.When the content of sample analysis firpene from evaporimeter A＜10%, stop the heating of evaporimeter A, cessation reaction.Open the dispensing valve V of evaporimeter A bottom
2, discharges material goes rectifying to separate, and material obtains the commodity terpinol by the rectifying separation, and the unreacted raw material of rectifying gained and solvent are reused among the Returning evaporimeter A again.
Because the boiling point of terpinol is high and do not form azeotropic mixture with other composition, therefore enrichment is concentrated gradually for the product terpinol among the evaporimeter A, and water, solvent and firpene azeotropic vaporization according to a certain percentage, and condensation in catalyst material basket D, reaction repeated also is back among the evaporimeter A.Because the special role of reaction distillation, the product of catalyst surface are continued the raw material condensate liquid washing of evaporation easily and hightail catalyst, and do not rest on the catalyst or back-mixing, make side reaction significantly reduce, product terpinol yield significantly improves.
Below provide the embodiment that utilizes the total reflux reaction distilling apparatus to catalyze and synthesize terpinol.
Embodiment 1:
Be raw material with turpentine oil and water, be solvent with the isopropyl alcohol, the mass ratio of turpentine oil, water and isopropyl alcohol is 5: 2: 3, evaporator temperature is set at 155 ℃, the temperature adjusting of reactor (catalyst material basket) is at 60～80 ℃, catalyst consumption is 7.5% of reaction raw materials consumption, and the reaction time is 6h.After the reaction, product is through simple rectifying desolventizing, and through gas chromatographic analysis, the conversion ratio that calculates firpene is 97.9%, and the total recovery of terpinol product is 79.8%, and the yield of alpha-terpineol is 49.4%.The GC-MS spectrogram of product is referring to Fig. 2.
Embodiment 2:
Being raw material with turpentine oil and water, is solvent with the isopropyl alcohol, and the mass ratio of turpentine oil, water and isopropyl alcohol is 5: 2: 3, evaporator temperature is set at 155 ℃, the temperature adjusting of reactor (catalyst material basket) is at 60～80 ℃, and catalyst consumption is 10% of reaction raw materials consumption, and the reaction time is 6h.After the reaction, product is through simple rectifying desolventizing, and through gas chromatographic analysis, the conversion ratio that calculates firpene is 98.7%, and the total recovery of terpinol product is 68.6%, and the yield of alpha-terpineol is 47.7%.
Embodiment 3:
Be raw material with turpentine oil and water, be solvent with the isopropyl alcohol, the mass ratio of turpentine oil, water and isopropyl alcohol is 5: 2: 3, evaporator temperature is set at 155 ℃, the temperature adjusting of reactor (catalyst material basket) is at 45～65 ℃, catalyst consumption is 7.5% of reaction raw materials consumption, and the reaction time is 6h.After the reaction, product is through simple rectifying desolventizing, and through gas chromatographic analysis, the conversion ratio that calculates firpene is 94.0%, and the total recovery of terpinol product is 61.0%, and the yield of alpha-terpineol is 38.9%.
Embodiment 4:
Be raw material with turpentine oil and water, be solvent with the isopropyl alcohol, the mass ratio of turpentine oil, water and isopropyl alcohol is 5: 2: 3, evaporator temperature is set at 155 ℃, the temperature adjusting of reactor (catalyst material basket) is at 70～80 ℃, catalyst consumption is 7.5% of reaction raw materials consumption, and the reaction time is 6h.After the reaction, product is through simple rectifying desolventizing, and through gas chromatographic analysis, the conversion ratio that calculates firpene is 98.67%, and the total recovery of terpinol product is 63.6%, and the yield of alpha-terpineol is 38.9%.
Embodiment 5:
Be raw material with turpentine oil and water, be solvent with the isopropyl alcohol, the mass ratio of turpentine oil, water and isopropyl alcohol is 5: 1.5: 3, evaporator temperature is set at 155 ℃, the temperature adjusting of reactor (catalyst material basket) is at 70～80 ℃, catalyst consumption is 7.5% of reaction raw materials consumption, and the reaction time is 6h.After the reaction, product is through simple rectifying desolventizing, and through gas chromatographic analysis, the conversion ratio that calculates firpene is 95.9%, and the total recovery of terpinol product is 34.0%, and the yield of alpha-terpineol is 20.9%.
Embodiment 6:
Be raw material with turpentine oil and water, be solvent with the isopropyl alcohol, the mass ratio of turpentine oil, water and isopropyl alcohol is 5: 2: 3.5, evaporator temperature is set at 155 ℃, the temperature adjusting of reactor (catalyst material basket) is at 70～80 ℃, catalyst consumption is 7.5% of reaction raw materials consumption, and the reaction time is 6h.After the reaction, product is through simple rectifying desolventizing, and through gas chromatographic analysis, the conversion ratio that calculates firpene is 99.6%, and the total recovery of terpinol product is 78.0%, and the yield of alpha-terpineol is 43.2%.
Claims (10)
1. the total reflux reaction distilling apparatus of a synthetic terpinol is characterized in that being provided with evaporimeter, evaporating column, condenser coil, catalyst material basket, heating jacket; Described evaporimeter is provided with high steam entrance, feed(raw material)inlet, hot water outlet, temperature sensor and control interface, pressure sensor and remote alarm interface and discharging opening; Described evaporimeter top is connected with evaporating column, catalyst material basket is located in the evaporating column, and condenser coil is located in the catalyst material basket and with catalyst and is contacted, and described evaporating column outside is provided with heating jacket and heat-insulation layer, the bottom of evaporating column is provided with hot water inlet, and the top of evaporating column is provided with hot water outlet; The condenser coil two ends are cooling water inlet and coolant outlet.
2. a kind of total reflux reaction distilling apparatus of synthetic terpinol according to claim 1 is characterized in that described feed(raw material)inlet is provided with the charging valve.
3. a kind of total reflux reaction distilling apparatus of synthetic terpinol according to claim 1 is characterized in that described discharging opening is provided with dispensing valve.
4. the method for a synthetic terpinol is characterized in that adopting the total reflux reaction distilling apparatus of synthetic terpinol according to claim 1, and its step is as follows:
1) condenser coil is put into catalyst material basket, again catalyst and θ ring stainless steel cloth filler mixed packing are gone in the catalyst material basket, and catalyst material basket is fixed in the evaporating column closed evaporating tower;
2) close dispensing valve, raw pine fuel-economizing, water and solvent are joined in the evaporimeter by the charging valve, close the charging valve;
3) evaporimeter is heated, make the evaporation of raw material and solvent and condensation in catalyst material basket, the condensate liquid contact catalyst carries out catalytic reaction; Because the evaporating column outer wall has heating jacket and heat-insulation layer, so only condensation in catalyst material basket of steam; The mixed liquor of raw material and solvent forms azeotropic in the evaporation process; Product in the catalyst material basket and unreacted raw material rely on gravity reflux at the bottom of the tower in the evaporimeter, and terpinol is deposited in the evaporimeter, and raw material and solvent evaporate azeotropic again, and condensation in catalyst material basket, react again; When the content of sample analysis firpene from evaporimeter＜10%, stop the heating of evaporimeter, cessation reaction, open the dispensing valve of base of evaporator, discharges material is carried out rectifying again and is separated, material obtains the terpinol product by the rectifying separation, and the unreacted raw material of rectifying gained and solvent are reused in the Returning evaporimeter again.
5. as the method for a kind of synthetic terpinol as described in the claim 4, it is characterized in that in step 1) that described catalyst adopts cationic ion-exchange resin.
6. as the method for a kind of synthetic terpinol as described in the claim 5, it is characterized in that it is Amberlyst15, Amberlyst35, Amberlyst36 cationic ion-exchange resin that described cationic ion-exchange resin is selected model for use.
7. as the method for a kind of synthetic terpinol as described in the claim 4, it is characterized in that in step 1) the voidage in the described catalyst material basket is 25%～35%.
8. as the method for a kind of synthetic terpinol as described in the claim 4, it is characterized in that in step 1) the loadings of described catalyst is 7%～10% of raw material gross mass by mass percentage.
9. as the method for a kind of synthetic terpinol as described in the claim 4, it is characterized in that in step 2) in, described solvent adopts the low-carbon (LC) alcohols, and the mass ratio of described turpentine oil, water, solvent can be 5: (1.5～2): (3～3.5).
10. as the method for a kind of synthetic terpinol as described in the claim 4, it is characterized in that in step 3) the purpose that described evaporating column outside is provided with heating jacket and heat-insulation layer is to avoid steam in the condensation of tower wall; Described condenser coil places catalyst material basket, by the flow of condensed water in the adjustment condenser coil and condensation and the reaction temperature in the temperature control catalyst material basket; Described catalytic reaction is in 6h, and the mass concentration of firpene can be less than 10% in the evaporimeter, and described product is separated through rectifying again, and unreacted raw material and solvent return the total reflux reaction distilling apparatus again and reuse; Mainly contain minor by-products such as citrene, terpinolene, amphene in the described product, namely can obtain the terpinol product by distillation operation.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107892640A (en) * | 2017-05-31 | 2018-04-10 | 怀集县长林化工有限责任公司 | A kind of α firpenes isomery prepares the preparation method of amphene |
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| CN101108788A (en) * | 2007-07-13 | 2008-01-23 | 中国林业科学研究院林产化学工业研究所 | Method of manufacturing high purity alpha-terpineol |
| CN101365531A (en) * | 2005-07-28 | 2009-02-11 | 杜邦公司 | Reactors, reactor assemblies, and production processes |
| CN103044202A (en) * | 2013-01-08 | 2013-04-17 | 江苏宏邦化工科技有限公司 | Preparation method of alpha-terpilenol |
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| JPH10287600A (en) * | 1997-04-16 | 1998-10-27 | Mitsubishi Chem Corp | Production of cyclohexanol |
| 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 |
| CN101365531A (en) * | 2005-07-28 | 2009-02-11 | 杜邦公司 | Reactors, reactor assemblies, and production processes |
| CN101108788A (en) * | 2007-07-13 | 2008-01-23 | 中国林业科学研究院林产化学工业研究所 | Method of manufacturing high purity alpha-terpineol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107892640A (en) * | 2017-05-31 | 2018-04-10 | 怀集县长林化工有限责任公司 | A kind of α firpenes isomery prepares the preparation method of amphene |
| CN107892640B (en) * | 2017-05-31 | 2020-10-27 | 怀集县长林化工有限责任公司 | Preparation method for preparing camphene by alpha-pinene isomerization |
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