CN105837435A - Method for preparing isoborneol ester through continuous esterification - Google Patents
Method for preparing isoborneol ester through continuous esterification Download PDFInfo
- Publication number
- CN105837435A CN105837435A CN201610254757.2A CN201610254757A CN105837435A CN 105837435 A CN105837435 A CN 105837435A CN 201610254757 A CN201610254757 A CN 201610254757A CN 105837435 A CN105837435 A CN 105837435A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- reaction
- esterification
- isoborneol ester
- flow reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/04—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing isoborneol ester through continuous esterification. The method comprises the following steps of: by taking camphene and acetic acid as raw materials, implementing continuous sterification by using a tube type oscillatory flow reactor, thereby obtaining the isoborneol ester. By adopting the method and a device disclosed by the invention, continuous production of the isoborneol ester can be achieved; as heterogeneous solid granules are taken as a catalyst and are in a fluidization state, the problems that a conventional intermittent process is poor in heat conduction, non-uniform in temperature, rich in side reaction and the like can be solved, good heat conduction can be achieved, and as reaction heat accumulation is prevented, the service life of the catalyst is prolonged, the reaction selectivity of the catalyst is improved, and the catalyst can be easily separated from a product; due to a special structure of the device for the method, the turbulence property of a flowing material is improved, mass and heat transfer in the reaction process is improved, the surface of the catalyst can be updated in time, and thus the reaction velocity and the raw material conversion rate can be increased. The method and the device are not only applicable to industrial production of isoborneol ester in fine chemical engineering, but also applicable to other similar solid-liquid two-phase exothermic reaction process.
Description
Technical field
The invention belongs to field of fine chemical, be more particularly to a kind of method that continuous esterification prepares compounding acetic isoborneol ester.
Background technology
Compounding acetic isoborneol ester can be used as spice owing to having delicate fragrance and pine Folium Cunninghamiae lanceolatae abnormal smells from the patient, is mainly used in cosmetics, disinfectant and air freshener etc.；Additionally, compounding acetic isoborneol ester is also the important intermediate of artificial camphor, due to the scarcity of natural camphor so that the synthesis as the compounding acetic isoborneol ester of intermediate the most increasingly comes into one's own.
Industrial compounding acetic isoborneol ester typically with camphene and acetic acid as raw material, is esterified under catalyst action and obtains.The catalyst type being theoretically utilized in this esterification process is various, it is contemplated that catalyst life, to factors such as equipment corrosion, environmental pollution and post processings, and current domestic industry metaplasia mainly uses sulfonate ion-exchange membrane and acid cation exchange resin in producing.But this esterification process uses batch still to operate mostly at present, there is production process route longer, labor intensity is big, and catalyst is fragile, product composition instability, and once through yield is low and the deficiency such as post processing difficulty.Therefore, the commercial process for compounding acetic isoborneol ester need to optimize further and perfect.
The continuous production technology research producing compounding acetic isoborneol ester about camphene esterification is few.It is catalyst that patent CN1036950A just proposed employing natural mordenite in 1989, method with fixed bed adverse current continuous esterification synthesis of acetic acid Isobornyl, though the method achieves continuous operation, but it is unstable to there is catalyst performance, by-product is difficult to separate, product yield and purity are low, and investment is big with energy consumption waits deficiency.Patent CN101372453A of 2008 discloses a kind of fixed bed continuous esterification process improving compounding acetic isoborneol ester yield by controlling catalyst water content, patent CN101921191A of 2010 proposes and uses fixed bed equally, and with synthesis of molecular sieve as catalyst, fixed bed reactors and catalyst that the two process uses have preferable conversion ratio and selectivity.But owing to this reaction is a stronger exothermic reaction, easily causing system poor heat radiation, bed temperature is uneven and causes by-product to increase；And employing solid catalyst, its surface is easily formed the product of high concentration and hinders the forward of this reversible reaction to move, and only upgrading in time of catalyst surface could improve this situation.But the fixed bed reactors that two above patent uses do not solve two above key issue.
The Oscillatory Flow Reactor that the present invention uses has good mass-and heat-transfer performance, and there is under certain oscillating condition good mixed effect, the most also can there is the residence time destribution of approximation laminar flow, therefore for a lot of chemical reactions, there is advantageous advantage.At present Oscillatory Flow Reactor applies four the most classical class chemical reactions to include suspension polymerisation, ferment, prepare biodiesel (CN103254997A), catalytic reaction (US20140066667 A1), and rarely has report in the research of solid-liquid two-phase reaction system.The esterification of present invention research is that a heat effect substantially and exists the system of solid catalyst, is badly in need of a kind of reactor with good heat transfer mass transfer effect and solves the problem that industry exists at present, and Oscillatory Flow Reactor is exactly a good selection.
Summary of the invention
It is an object of the invention to provide a kind of method that continuous esterification prepares compounding acetic isoborneol ester, the by-product which overcoming the existence of existing technique is many, reaction rate is slow, catalyst easily inactivates because of moisture and polymer, the problems such as heat transfer is the best with mass transfer, the method can realize the good catalytic effect of catalyst and the life-span is long；Reactor is owing to using special construction to have prominent heat transfer and mass transfer ability, and its interior temperature distribution uniform, controllable, catalyst surface realizes upgrading in time, and reaction rate is accelerated, selectivity advantages of higher.
For achieving the above object, technical scheme is as follows:
A kind of continuous esterification prepares the method for compounding acetic isoborneol ester and device includes the process of continuous esterification and realizes equipment two parts of this process, specifically comprises the following steps that
The process of described continuous esterification is to be successively inputted to according to a certain percentage be mounted with in the Oscillatory Flow Reactor of solid catalyst react by material camphene and acetic acid, controls certain process conditions, obtains target product compounding acetic isoborneol ester.
Described process apparatus refers to comprise Oscillatory Flow Reactor, clapp oscillator, raw material mixing channel, a series of equipment of the continuous esterification process that realizes of the equipment compositions such as purification of products tower, wherein Oscillatory Flow Reactor (see accompanying drawing 2) is to realize the reactor that esterification process is main, course of reaction gives the material in reactor with the vibration of some strength by clapp oscillator (CN201520229309.8), makes the catalyst in reactor present uniform fluidized suspension state.
Particularly as follows:
(1) with industry camphene and industrial acetic as raw material, be separately input in raw material mixing channel V-101 by certain mol proportion, stir, and utilize steam or hot water by raw material preheating to 30 ~ 50 DEG C；
(2) the raw material pump P-101A/B after preheating is delivered to be mounted with in shell and tube Oscillatory Flow Reactor R-101 of solid catalyst；Open oscillation generator P-102, carry out esterification；The heat of Oscillatory Flow Reactor is shifted by heat transferring medium in tube side；
(3) esterification reaction product stores to product storage tank V-102, then is delivered to purification of products tower T-101 by pump P-103 A/B, after overhead product is purified, then is delivered to product storage tank V-103 by pump P-104 A/B.
In step (1), the mol ratio of industry camphene and industrial acetic is 1:1.1 ~ 2.0.
The solid catalyst described in step (2) one in zeolite molecular sieve, solid super-strong acid, heteropoly acid and cation exchange resin；Solid catalyst loadings is the 10 ~ 30% of reactor volume.
In step (2), the condition of esterification is: reaction temperature 20 ~ 100 DEG C, and industrial acetic, the air speed of industry camphene are 0.1 ~ 6.0h-1, reaction pressure is 0.1
MPa~1.0MPa。
The amplitude of step (2) shell and tube Oscillatory Flow Reactor is 1 ~ 20mm, and frequency is 1 ~ 5Hz, and vibrate Reynolds numberRe oFor 800-2500, clean Reynolds numberRe nFor 800-1000, speed ratioψFor 1-2, make catalyst present uniformly and fluidize state.
The quantity of the shell and tube Oscillatory Flow Reactor described in step (2) is one or more parallel connection.
The inner member of the shell and tube Oscillatory Flow Reactor described in step (2) is the one in baffle plate, periodic expansion joint, screw rod.
The feature of the device (accompanying drawing 1) that the method is used is:
Be transported to the shell and tube Oscillatory Flow Reactor (accompanying drawing 2) of one or more parallel connection after material camphene and acetic acid are squeezed into raw material mixing channel by fluid delivery pump, reactor is built with certain solid catalyst；The amplitude of this reactor is controlled by clapp oscillator (CN201520229309.8), and frequency of oscillation is controlled by converter regulation, and both cooperations make the reciprocating vibration under certain amplitude and frequency of the material in reactor, it is ensured that catalyst is in and fluidizes state uniformly；The heat of reactor is shifted by shell side heat transferring medium, it is ensured that reaction temperature uniformly and is unlikely to too high；The esterification products of reactor outlet enters last purification of products tower and purifies.
Vibration fluid bed was used for reducing the critical fludization velocity of solid particle in the past, applies being dried at solid particle, and has the advantages that amplitude is little, frequency is high, and how not parallel orientation of oscillation is with gravity direction.And herein described oscillatory flow gasifying device amplitude is far above being dried by, frequency far below vibration fluid bed, can be used for improving heat transfer, solid-liquid mass transfer and strengthening mixing；It is embodied in:
First, owing to material and catalyst present vibration and suspended state in reactor, and whole beds is evenly distributed on radial and axial, heat-transfer effect is better than fixed bed and suspension bed, it is possible not only to make the uniformity of temperature profile of reaction system, the heat that simultaneously can in time this exothermic reaction be produced is transferred out in time, it is not easy to produce heat accumulation, effectively prevent by-product camphene polymer and the generation of different camphane ester, in addition reactant whole bed axially on close to laminar flow, the time of staying is homogeneous, thus reaction selectivity is higher, feed stock conversion is high, by-product is few, product quality is stable；
Secondly, there is a considerable amount of inner member in Oscillatory Flow Reactor, when the external world applies some strength vibration, the position between adjacent inner member can form eddy-currents, is equivalent to full mixing reactor the most diametrically, and therefore between material, mass transfer is good.For catalyst and reactant, owing to mixability is more preferable, the contact probability of reactant and catalytic active center is bigger, then reaction rate is faster；For catalyst self, owing to reaction may generate camphene polymer and be attached to catalyst active center, when there is vibration in system, then catalyst surface is constantly washed away by material, it is not easy to be adhered to by polymer, and surface can upgrade in time, the product generated at catalyst surface can be made to spread in time, the forward not interfering with esterification is carried out.Therefore, the good mass-transfer of Oscillatory Flow Reactor, can make catalyst effect more preferably and life, reaction rate is accelerated, and conversion per pass uprises；
Again, the oscillation intensity of reactor can be adjusted by adjusting amplitude and frequency, heat effect according to different reactant air speeds or different exothermic reaction can get the vibration Reynolds number of respective range, clean Reynolds number and speed ratio, catalyst is made to be in preferable even fluidizing state, the reaction unit suitability and operating flexibility are bigger, this device i.e. is not only available for the synthesis of compounding acetic isoborneol ester, it is also possible to for the reaction that other heat effects are bigger.
Compared with prior art, it is an advantage of the current invention that:
1) the shell and tube Oscillatory Flow Reactor that the present invention uses, owing to it can significantly improve the mixability of material, mass-and heat-transfer function admirable, and technical process is easily controlled, there is under continuous operation state excellent residence time destribution characteristic, chemical process industry has shown huge industrial application value.There is maximum problem and be that heat transfer, mass transfer and catalysqt deactivation in current industrial production compounding acetic isoborneol ester, uses shell and tube Oscillatory Flow Reactor the most just to solve above three big problems；
2) Oscillatory Flow Reactor is applied in camphene esterification reaction by the present invention, it is first this reactor to be applied in the solid-liquid two-phase system reaction of bigger solid particle, not only achieve continuous prodution, and solving uneven and different camphane ester (by-product) too high levels problem of dispelling the heat, the selectivity of camphene and the life-span of catalyst are much better than common fixed bed reactors or suspension bed；In addition this device is applied equally to other solid-liquid two phase reaction, by keeping the solids at vibration and suspended state, is i.e. remarkably improved the effectiveness that solid material participates in reaction.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that compounding acetic isoborneol ester method is prepared in serialization of the present invention；
Wherein: V-101 is raw material mixing channel；R-101 is shell and tube Oscillatory Flow Reactor；V-102 is product storage tank；T-101 is purification of products tower；V-103 is product storage tank；P-101A/B, P-103 A/B, P-104 A/B is material-handling pump；P-102 is oscillation generator；
Fig. 2 is shell and tube Oscillatory Flow Reactor of the present invention, wherein: a is vibration mouth；B, e are drain；C, d are followed successively by the export and import of material；F is row's mouth；G, h are followed successively by the export and import of recirculated water.
Detailed description of the invention
By describing the technology contents of the present invention, structural feature in detail, being realized purpose and effect; and combine detailed description of the invention and coordinate accompanying drawing to describe in detail; but protection scope of the present invention is not limited to specific examples below, this device is applied to other similar solid-liquid biphase exothermic reaction systems and also belongs to this patent scope.
A kind of continuous esterification is prepared the method for compounding acetic isoborneol ester and is included the process of continuous esterification and realize equipment two parts of this process, specifically comprises the following steps that
The process of described continuous esterification is to continuously enter according to a certain percentage to be mounted with in the Oscillatory Flow Reactor of solid catalyst by material camphene and acetic acid to react, and controls certain process conditions, obtains target product compounding acetic isoborneol ester.
Described process apparatus refers to comprise Oscillatory Flow Reactor, clapp oscillator, raw material mixing channel, a series of equipment of the continuous esterification process that realizes of the equipment compositions such as purification of products tower, wherein Oscillatory Flow Reactor (see accompanying drawing 2) is to realize the reactor that esterification process is main, course of reaction gives the material in reactor with the vibration of some strength by clapp oscillator (CN201520229309.8), makes the catalyst in reactor present uniform fluidized suspension state.
Described industrial camphene and the mol ratio of industrial acetic are 1:1.1 ~ 2.0.
Described solid catalyst one in zeolite molecular sieve, solid super-strong acid, heteropoly acid and cation exchange resin；Solid catalyst loadings is the 10 ~ 30% of reactor volume.
The condition of described esterification is: reaction temperature 20 ~ 100 DEG C, and industrial acetic, the air speed of industry camphene are 0.1 ~ 6.0h-1, reaction pressure is 0.1 MPa ~ 1.0MPa.
The amplitude of described shell and tube Oscillatory Flow Reactor is 1 ~ 20mm, and frequency is 1 ~ 5Hz, and vibrate Reynolds numberRe oFor 800-2500, clean Reynolds numberRe nFor 800-1000, speed ratioψFor 1-2, make catalyst present uniformly and fluidize state.
The quantity of described shell and tube Oscillatory Flow Reactor is one or more parallel connection.
The inner member of described shell and tube Oscillatory Flow Reactor is the one in baffle plate, periodic expansion joint, screw rod.
Embodiment
1
With industry camphene and industrial acetic as raw material, stir after being squeezed into raw material mixing channel V-101 respectively by the mol ratio of 1:1.1, and utilize hot water by raw material preheating to 40 DEG C；Raw material pump after preheating is got in single tubulation Oscillatory Flow Reactor with the flow velocity of 3.18ml/s.This reactor uses the inner member of annulus baffle-type, internal equipped with 10%(reactor volume) NKC-9 cation exchange resin, resin uses reaction raw materials to soak in advance, utilizes constant temperature water bath reaction temperature to be controlled at 40 ± 1 DEG C, and reaction pressure is normal pressure.Opening oscillation generator, original frequency is set to 20HZ, after the full reactor of catalyst distribution, frequency is adjusted to 3 Hz, and amplitude is 7mm, and now catalyst can be uniformly distributed in reactor；Carry out esterification, and purified after, obtain product.
Camphene selectivity 98.7% with this understanding, the yield of compounding acetic isoborneol ester is 83.9%, and in product, the content of side reaction gained different camphane ester is 0.13%(mass fraction, lower with), catalyst continuous service life is more than 60 days；Under equal conditions, the camphene selectivity 92.5% of batch tank reaction, the yield of compounding acetic isoborneol ester is 65.3%, and in product, the content of side reaction gained different camphane ester is 0.66%, and catalyst continuous service life was at about 30 days.
Embodiment
2
With industry camphene and industrial acetic as raw material, stir after being squeezed into raw material mixing channel V-101 respectively by the mol ratio of 1:1.1, and utilize hot water by raw material preheating to 50 DEG C；Raw material pump after preheating is got in single tubulation Oscillatory Flow Reactor with the flow velocity of 3.18ml/s.This reactor uses the inner member of annulus baffle-type, internal equipped with 10%(reactor volume) NKC-9 cation exchange resin, resin uses reaction raw materials to soak in advance, utilizes constant temperature water bath reaction temperature to be controlled at 50 ± 1 DEG C, and reaction pressure is normal pressure.Opening oscillation generator, original frequency is set to 20HZ, after the full reactor of catalyst distribution, frequency is adjusted to 3 HZ, and amplitude is 7mm, and now catalyst can be uniformly distributed in reactor；Carry out esterification, and purified after, obtain product.
Camphene selectivity 96.9% with this understanding, the yield of compounding acetic isoborneol ester is 80.4%, and in product, the content of side reaction gained different camphane ester is 0.54%, and catalyst continuous service life is more than 60 days；Under equal conditions, the camphene selectivity 89.2% of batch tank reaction, the yield of compounding acetic isoborneol ester is 63.5%, and in product, the content of side reaction gained different camphane ester is 1.90%, and catalyst continuous service life was at about 30 days.
Embodiment
3
With industry camphene and industrial acetic as raw material, stir after being squeezed into raw material mixing channel V-101 respectively by the mol ratio of 1:2, and utilize hot water by raw material preheating to 40 DEG C；Raw material pump after preheating is got in single tubulation Oscillatory Flow Reactor with the flow velocity of 3.18ml/s.This reactor uses the inner member of annulus baffle-type, internal equipped with 10%(reactor volume) NKC-9 cation exchange resin, resin uses reaction raw materials to soak in advance, utilizes constant temperature water bath reaction temperature to be controlled at 40 ± 1 DEG C, and reaction pressure is normal pressure.Opening oscillation generator, original frequency is set to 20Hz, after the full reactor of catalyst distribution, frequency is adjusted to 3 Hz, and amplitude is 7mm, and now catalyst can be uniformly distributed in reactor；Carry out esterification, and purified after, obtain product.
Camphene selectivity 99.1% with this understanding, the yield of compounding acetic isoborneol ester is 88.4%, and in product, the content of side reaction gained different camphane ester is 0.09%, and catalyst continuous service life is more than 45 days；Under the same terms, the camphene selectivity 93.8% of batch tank reaction, the yield of compounding acetic isoborneol ester is 69.5%, and in product, the content of side reaction gained different camphane ester is 0.35%, and catalyst continuous service life was at about 25 days.
By above case result it can be seen that use the result of methods and apparatus of the present invention gained to be much better than batch process.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.
Claims (7)
1. the method that a continuous esterification prepares compounding acetic isoborneol ester, it is characterised in that: comprise the following steps:
(1) with industry camphene and industrial acetic as raw material, be separately input in raw material mixing channel V-101 by certain mol proportion, stir, and utilize steam or hot water by raw material preheating to 30 ~ 50 DEG C；
(2) the raw material pump P-101A/B after preheating is delivered to be mounted with in shell and tube Oscillatory Flow Reactor R-101 of solid catalyst；Open oscillation generator P-102, carry out esterification；The heat of Oscillatory Flow Reactor is shifted by heat transferring medium in tube side；
(3) esterification reaction product stores to product storage tank V-102, then is delivered to purification of products tower T-101 by pump P-103 A/B, after overhead product is purified, then is delivered to product storage tank V-103 by pump P-104 A/B.
Continuous esterification the most according to claim 1 prepares the method for compounding acetic isoborneol ester, it is characterised in that: in step (1), the mol ratio of industry camphene and industrial acetic is 1:1.1 ~ 2.0.
Continuous esterification the most according to claim 1 prepares the method for compounding acetic isoborneol ester, it is characterised in that: the one in zeolite molecular sieve, solid super-strong acid, heteropoly acid and cation exchange resin of the solid catalyst described in step (2)；Solid catalyst loadings is the 10 ~ 30% of reactor volume.
Continuous esterification the most according to claim 1 prepares the method for compounding acetic isoborneol ester, it is characterised in that: in step (2), the condition of esterification is: reaction temperature 20 ~ 100 DEG C, and industrial acetic, the air speed of industry camphene are 0.1 ~ 6.0h-1, reaction pressure is 0.1 MPa ~ 1.0MPa.
Continuous esterification the most according to claim 1 prepares the method for compounding acetic isoborneol ester, it is characterised in that: the amplitude of step (2) shell and tube Oscillatory Flow Reactor is 1 ~ 20mm, and frequency is 1 ~ 5Hz, and vibrate Reynolds numberRe oIt is 800 ~ 2500, clean Reynolds numberRe nIt is 800 ~ 1000, speed ratioψIt is 1 ~ 2.
Continuous esterification the most according to claim 1 prepares the method for compounding acetic isoborneol ester, it is characterised in that: the quantity of the shell and tube Oscillatory Flow Reactor described in step (2) is one or more parallel connection.
Continuous esterification the most according to claim 1 prepares the method for compounding acetic isoborneol ester, it is characterised in that: the inner member of the shell and tube Oscillatory Flow Reactor described in step (2) is the one in baffle plate, periodic expansion joint, screw rod.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610254757.2A CN105837435B (en) | 2016-04-25 | 2016-04-25 | A kind of method that continuous esterification prepares compounding acetic isoborneol ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610254757.2A CN105837435B (en) | 2016-04-25 | 2016-04-25 | A kind of method that continuous esterification prepares compounding acetic isoborneol ester |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105837435A true CN105837435A (en) | 2016-08-10 |
| CN105837435B CN105837435B (en) | 2018-10-30 |
Family
ID=56590165
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610254757.2A Active CN105837435B (en) | 2016-04-25 | 2016-04-25 | A kind of method that continuous esterification prepares compounding acetic isoborneol ester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105837435B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103908944A (en) * | 2012-12-30 | 2014-07-09 | 灯塔北方化工有限公司 | High-pressure alcoholysis device |
| CN112250572A (en) * | 2020-11-17 | 2021-01-22 | 广西壮族自治区林业科学研究院 | Method for synthesizing bornyl acetate from turpentine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276453A (en) * | 2011-06-30 | 2011-12-14 | 福州大学 | Method for preparing isobomyl acetate through camphene esterification |
| CN104478666A (en) * | 2014-08-25 | 2015-04-01 | 福州大学 | Method for preparing isoborneol through continuous saponification of isobornyl acetate |
-
2016
- 2016-04-25 CN CN201610254757.2A patent/CN105837435B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276453A (en) * | 2011-06-30 | 2011-12-14 | 福州大学 | Method for preparing isobomyl acetate through camphene esterification |
| CN104478666A (en) * | 2014-08-25 | 2015-04-01 | 福州大学 | Method for preparing isoborneol through continuous saponification of isobornyl acetate |
Non-Patent Citations (2)
| Title |
|---|
| 张龙等: "《绿色化学》", 31 August 2014 * |
| 赵海泉等: "莰烯酯化连续化工艺的研究", 《安徽化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103908944A (en) * | 2012-12-30 | 2014-07-09 | 灯塔北方化工有限公司 | High-pressure alcoholysis device |
| CN112250572A (en) * | 2020-11-17 | 2021-01-22 | 广西壮族自治区林业科学研究院 | Method for synthesizing bornyl acetate from turpentine |
| CN112250572B (en) * | 2020-11-17 | 2023-03-10 | 广西壮族自治区林业科学研究院 | Method for synthesizing bornyl acetate from turpentine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105837435B (en) | 2018-10-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Ma et al. | Photocatalytic conversion of biomass-based monosaccharides to lactic acid by ultrathin porous oxygen doped carbon nitride | |
| CN101978031A (en) | Method and device for producing synthesis gas from biomass | |
| CN107935846A (en) | A kind of apparatus and method of continuous production environment-friendlyplasticizer plasticizer | |
| CN103611487B (en) | Impinging stream reactor | |
| CN101486919A (en) | Sectional temperature-controlled fluidized bed type biomass rapid pyrolysis reactor | |
| CN105837435A (en) | Method for preparing isoborneol ester through continuous esterification | |
| CN108467024B (en) | Fluidized bed for batch preparation of carbon nanotubes based on chemical vapor deposition method | |
| CN1958146A (en) | Multiple stage fluidized-bed reactor and method for synthesizing chloroethylene | |
| CN102001668B (en) | Silicon tetrachloride hydrogenation reactor introducing microcirculation distribution structure | |
| CN106635114A (en) | Device and method for realizing co-production of catalytic cracking oil gas by waste rubber powder in fluidized state | |
| CN101537328A (en) | Raw material gas intake method for fluidized bed | |
| CN101219920A (en) | Ethanol Dehydration Process Using Molecular Sieve Catalyst | |
| CN101759819B (en) | Device for preparing chlorosulfonated polyethylene by gas-solid phase method | |
| CN202671471U (en) | Device for preparing chlorinated polyvinyl chloride by plasma gas solid phase method | |
| CN102161718B (en) | Method and device for continuously producing chlorinated polyvinyl chloride by low-temperature plasma circulating bed | |
| CN111111562B (en) | Aromatic ammoxidation combined fluidized bed reaction device and reaction method thereof | |
| CN110240197A (en) | The Multilevel B iOCl microballoon of ultrathin nanometer piece self assembly and its photocatalysis be coupled benzylamine to imines application | |
| CN104096519B (en) | Fluidized-bed reactor and its application | |
| CN102276453A (en) | Method for preparing isobomyl acetate through camphene esterification | |
| CN207463192U (en) | Fluid bed reaction apparatus | |
| CN1137769C (en) | Synthesizing slurry-bed reactor | |
| CN111170845B (en) | Method for producing lactic acid by catalytic conversion of glucose and application thereof | |
| CN104607114B (en) | Apparatus and process for producing chlorinated high polymer | |
| CN103145904B (en) | Uniform ion exchange resin granule production equipment | |
| CN221753242U (en) | System for preparing catalyst by internal circulation reinforced spouted pyrolysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |