CN115403445B - Preparation method of dihydromyrcenol - Google Patents
Preparation method of dihydromyrcenol Download PDFInfo
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- CN115403445B CN115403445B CN202211127038.6A CN202211127038A CN115403445B CN 115403445 B CN115403445 B CN 115403445B CN 202211127038 A CN202211127038 A CN 202211127038A CN 115403445 B CN115403445 B CN 115403445B
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- dihydromyrcene
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- XSNQECSCDATQEL-UHFFFAOYSA-N dihydromyrcenol Chemical compound C=CC(C)CCCC(C)(C)O XSNQECSCDATQEL-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229930008394 dihydromyrcenol Natural products 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 44
- FUDNBFMOXDUIIE-UHFFFAOYSA-N 3,7-dimethylocta-1,6-diene Chemical compound C=CC(C)CCC=C(C)C FUDNBFMOXDUIIE-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002253 acid Substances 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006703 hydration reaction Methods 0.000 claims abstract description 5
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims description 15
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 11
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 9
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000012824 chemical production Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000002699 waste material Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 239000003205 fragrance Substances 0.000 description 3
- 239000011973 solid acid Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 241000207199 Citrus Species 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 241000218691 Cupressaceae Species 0.000 description 1
- 244000178870 Lavandula angustifolia Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/03—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2
- C07C29/04—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by addition of hydroxy groups to unsaturated carbon-to-carbon bonds, e.g. with the aid of H2O2 by hydration of carbon-to-carbon double bonds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical production, and in particular discloses a preparation method of dihydromyrcenol, which comprises the following steps: the liquid acid is fully contacted with the reaction liquid under the action of the emulsifying agent, the dihydromyrcene and the water are subjected to hydration reaction under the catalysis of the liquid acid to generate dihydromyrcene alcohol, an ultrasonic generator is adopted in the reaction process to generate ultrasonic waves to strengthen mass transfer in the reaction process, the reaction liquid is separated after the reaction is finished, and the liquid acid is applied to the next batch of reaction. The method has the advantages of high yield, high conversion rate, high reaction rate, easy separation of reaction products, low energy consumption and simple process, and is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a preparation method of dihydromyrcenol.
Background
The chemical formula of the dihydromyrcenol is C10H20O, and the English name is: dihydromyrcenol, CAS number: 53219-21-9, colorless slightly thick liquid. The relative density is 0.830-0.837, the refractive index is 1.439-1.443, the flash point is 79 ℃, the boiling point is 78 ℃/1333.2Pa, colorless liquid is insoluble in water, is soluble in 4-6 volume percent of 55 percent ethanol or 1-2 volume percent of 70 percent ethanol, and is also soluble in oily perfume. The fragrance is fresh, sweet and powerful, has fresh and spicy citrus, pine and cypress, lavender, fruit fragrance and flower fragrance, is sweet and sour, and has white lemon and cologne smell.
The dihydromyrcenol is one of the downstream products of the turpentine deep processing group, is also a large amount of perfume commonly used internationally, is widely applied to soaps, detergents and other daily industrial products, has a global demand of more than 1 ten thousand tons in recent years, and is continuously increasing due to the continuous popularity of characteristic aroma.
In the prior art, two main synthetic routes of dihydromyrcene exist:
The first category is direct hydration, which uses liquid acid as catalyst, but has the problems of long reaction time, low selectivity, etc., and the process generates a large amount of waste acid. The related process using solid acid and resin as catalyst has the problem of using a large amount of solvent because water is a strong polar solvent, and dihydromyrcene is a nonpolar solvent, if no solvent or a small amount of solvent is added, the dihydromyrcene becomes three-phase reaction when contacting with the solid acid, the reaction efficiency is extremely low, only a large amount of solvent is added to change the dihydromyrcene into homogeneous phase and then react with the solid acid or the acid resin, a large amount of solvent is necessarily used in the process, the solvent is distilled and removed after purification, a large amount of energy is consumed, and the dihydromyrcene occupies a small proportion due to the addition of a large amount of solvent, and the reaction time is about 50 hours. Thus, the production efficiency is extremely low.
The other general category is an indirect hydration method, wherein after the residual carboxylic acid of the dihydromyrcene is subjected to addition esterification under the catalysis of acid, alkali is used to react with the esterified dihydromyrcene, and corresponding carboxylate and dihydromyrcene alcohol are generated in the saponification reaction process. The process has complicated reaction steps, and generates a large amount of waste carboxylate, thereby generating a large amount of waste salt.
Therefore, the field needs to develop a novel process which has the advantages of efficient reaction, reduced energy consumption, improved yield, simple process and easy industrialized production of the dihydromyrcenol.
Disclosure of Invention
The invention aims to provide a preparation method of dihydromyrcenol, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for preparing dihydromyrcenol, which comprises the following steps:
Step one: preparing an emulsifier, wherein the emulsifier comprises a polyethylene glycol 600 emulsifier, an OP10 emulsifier, fatty alcohol polyoxyethylene ether and octadecylamine polyoxyethylene ether;
Step two: adding an emulsifying agent, liquid acid and dihydromyrcene into a reaction kettle, increasing the reaction contact area between the liquid acid and the dihydromyrcene under the emulsification action of the emulsifying agent, and maintaining the reaction temperature at 40-100 ℃ to generate hydration reaction between the dihydromyrcene and water to generate dihydromyrcene alcohol;
step three: an ultrasonic generator is adopted in the reaction process to generate ultrasonic waves to strengthen the mass transfer efficiency, so that the reaction time is shortened;
Step four: and (3) after the reaction is finished, carrying out post-treatment on the materials, separating the liquid acid from the reaction products by a butterfly type centrifugal machine, carrying out alkaline washing on the products, carrying out rectification, separation and purification on the products, diluting the liquid acid with water to the technological requirements, and then recycling the liquid acid.
Based on the technical scheme, the invention also provides the following optional technical schemes:
in one alternative: the emulsifier is selected from the following group: one or more of polyethylene glycol 600 emulsifier, OP10 emulsifier, fatty alcohol polyoxyethylene ether and octadecylamine polyoxyethylene ether are mixed for use; the liquid acid is selected from the group consisting of: one or more of trifluoromethanesulfonic acid and methanesulfonic acid are used in combination.
In one alternative: in the second step, the reaction time is 24 to 54 hours, preferably 24 hours, more preferably 25 hours.
In one alternative: in said step two, the temperature of said reaction is 40-100 ℃, preferably 60-85 ℃, more preferably 70-95 ℃, most preferably 80-82 ℃.
In one alternative: in the second step, the mass ratio of the dihydromyrcene to the liquid acid is 1:2 or 1:1.8 or 1:1.5.
In one alternative: in the second step, the emulsifier is polyethylene glycol 600 emulsifier, and the dosage of the emulsifier is as follows;
The mass ratio of the polyethylene glycol 600 emulsifier to the dihydromyrcene is as follows: polyethylene glycol 600 emulsifier: dihydromyrcene=0.02-0.005: 1 or 0.01-0.02:1 or 0.015-0.02:1;
In one alternative: the emulsifier is OP10 emulsifier, and the mass ratio of the emulsifier to the dihydromyrcene is as follows: OP10 emulsifier: dihydromyrcene=0.015-0.008: 1 or 0.01-0.015:1 or 0.008-0.0014:1;
The mass ratio of the octadecylamine polyoxyethylene ether to the dihydromyrcene is that the octadecylamine polyoxyethylene ether is that the dihydromyrcene=0.03-0.015: 1 or 0.03-0.02:1 or 0.02-0.015:1.
In one alternative: in the second step, the concentration of the liquid acid comprises the concentrations of the aqueous solutions corresponding to the various acids;
the concentration (mass fraction) of the trifluoromethanesulfonic acid is 5% -55%, preferably 10% -50%, more preferably 15% -20%.
The concentration (mass fraction) of the methylsulfonic acid is 30% -70%, preferably 30% -50%, more preferably 50% -70%.
In one alternative: the recovery treatment comprises separating oil phase (crude dihydromyrcenol) and water phase (liquid acid) from the reacted emulsion by a centrifuge, performing alkaline washing on the oil phase, separating and purifying by rectification, and diluting the liquid acid with water to the target requirement.
Compared with the prior art, the invention has the following beneficial effects:
The emulsifier is adopted to increase the contact area mass transfer of the liquid acid and the dihydromyrcene, so that the reaction rate is improved by 1-2 times. The catalyst adopts liquid acid (trifluoromethanesulfonic acid, methanesulfonic acid) and has high catalytic activity and low cost. Avoiding a great deal of energy consumption and waste caused by using a great deal of solvent in the related process of the solid catalyst. The selectivity is far higher than that of the traditional catalyst sulfuric acid and phosphoric acid, and the production cost is greatly reduced. The reaction liquid is vibrated by adopting ultrasonic waves, so that the reaction efficiency is further improved, and the reaction time is shortened. The adoption of a disc type centrifuge to separate the liquid acid from the emulsifier avoids the addition of a large amount of alkali for neutralization, and avoids the generation of waste salt and waste acid. Meanwhile, the application of liquid acid is realized, and the production cost and the three-waste treatment cost are reduced. As the reaction rate is increased, the contact time of the product, the reaction raw material and the catalyst is reduced, and the reaction selectivity is improved.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent.
Example 1
Dihydromyrcene: 15% of trifluoromethanesulfonic acid (mass fraction): polyethylene glycol 600 emulsifier in mass ratio=1:1.5: 0.018, and adding into a reaction kettle in any order, wherein the reaction temperature is as follows: the reaction time is 25h at 81 ℃, the reaction efficiency is promoted by adopting ultrasonic oscillation in the reaction process, the emulsion is pumped into a disc centrifuge to separate the reaction solution from the liquid acid after the reaction is finished, the separated liquid acid is diluted to the concentration required by the process and then is used, the reaction solution is subjected to alkaline washing and then is rectified (the mode of treating the reactant after the reaction is finished is consistent with that of the follow-up examples 2-10, and therefore, the follow-up reactant treatment process is not repeated). Under the condition, the conversion rate is 92% and the selectivity is more than 91%.
Example 2
Dihydromyrcene: 65% of methylsulfonic acid (mass fraction): polyethylene glycol 600 emulsifier in mass ratio=1:1.5: 0.018, and adding into a reaction kettle in any order, wherein the reaction temperature is as follows: the reaction process adopts ultrasonic oscillation to promote the reaction efficiency at 81 ℃ for 25 hours, and the conversion rate is 90% and the selectivity is more than 93% under the condition.
Example 3
Dihydromyrcene: 15% of trifluoromethanesulfonic acid (mass fraction): OP10 emulsifier in mass ratio=1:1.5: 0.01 is put into a reaction kettle in any order, the reaction process adopts ultrasonic oscillation to promote the reaction efficiency, and the reaction temperature is as follows: the reaction time is 25 hours at 81 ℃, and the conversion rate is 86% and the selectivity is more than 90% under the condition.
Example 4
Dihydromyrcene: 65% of methylsulfonic acid (mass fraction): OP10 emulsifier in mass ratio=1:1.5: 0.01 is put into a reaction kettle in any order, the reaction process adopts ultrasonic oscillation to promote the reaction efficiency, and the reaction temperature is as follows: the reaction time is 25 hours at the temperature of 81 ℃, and the conversion rate is 89% and the selectivity is more than 92% under the condition.
Example 5
Dihydromyrcene: 15% of trifluoromethanesulfonic acid (mass fraction): peregal emulsifier in mass ratio=1:1.5: 0.008 are put into a reaction kettle in any order, the reaction process adopts ultrasonic oscillation to promote the reaction efficiency, and the reaction temperature is as follows: the reaction time is 25 hours at the temperature of 81 ℃, and the conversion rate is 91% under the condition, and the selectivity is more than 93%.
Example 6
Dihydromyrcene: 65% of methylsulfonic acid (mass fraction): peregal emulsifier in mass ratio=1:1.5: 0.01 is put into a reaction kettle in any order, the reaction process adopts ultrasonic oscillation to promote the reaction efficiency, and the reaction temperature is as follows: the reaction time is 25 hours at the temperature of 81 ℃, and the conversion rate is 89% under the condition, and the selectivity is more than 93%.
Example 7
Dihydromyrcene: 15% of trifluoromethanesulfonic acid (mass fraction): octadecylamine polyoxyethylene ether emulsifier in mass ratio=1:1.5: 0.02 into a reaction kettle in any order, wherein the reaction process adopts ultrasonic oscillation to promote the reaction efficiency, and the reaction temperature is as follows: the reaction time is 25 hours at 81 ℃, and the conversion rate under the condition is 92 percent, and the selectivity is more than 91 percent.
Example 8
Dihydromyrcene: 65% of methylsulfonic acid (mass fraction): octadecylamine polyoxyethylene ether emulsifier in mass ratio=1:1.5: 0.02 into a reaction kettle in any order, wherein the reaction process adopts ultrasonic oscillation to promote the reaction efficiency, and the reaction temperature is as follows: the reaction time is 25 hours at the temperature of 81 ℃, and the conversion rate is 90% and the selectivity is more than 92% under the condition.
The foregoing is merely specific embodiments of the disclosure, but the protection scope of the disclosure is not limited thereto, and any person skilled in the art can easily think about changes or substitutions within the technical scope of the disclosure, and it is intended to cover the scope of the disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (9)
1. The preparation method of the dihydromyrcenol is characterized by comprising the following steps of:
step one: preparing an emulsifying agent;
Step two: adding an emulsifying agent, liquid acid and dihydromyrcene into a reaction kettle, increasing the reaction contact area between the liquid acid and the dihydromyrcene under the emulsification action of the emulsifying agent, and maintaining the reaction temperature at 40-100 ℃ to generate hydration reaction between the dihydromyrcene and water to generate dihydromyrcene alcohol;
step three: an ultrasonic generator is adopted in the reaction process to generate ultrasonic waves to strengthen the mass transfer efficiency, so that the reaction time is shortened;
step four: after the reaction is finished, carrying out post-treatment on the materials, separating liquid acid from reaction products by a butterfly type centrifuge, carrying out alkaline washing on the products, and then, carrying out rectification, separation and purification on the products, diluting the liquid acid with water to the technological requirements, and then, recovering the liquid acid;
The emulsifier is selected from the group consisting of: one or more of polyethylene glycol 600 emulsifier, OP10 emulsifier, fatty alcohol polyoxyethylene ether and octadecylamine polyoxyethylene ether are mixed for use; the liquid acid is trifluoromethanesulfonic acid or methanesulfonic acid.
2. The method for producing dihydromyrcenol as claimed in claim 1, wherein in the second step, the reaction time is 24 to 54 hours.
3. The method for producing dihydromyrcenol as claimed in claim 2, wherein in the second step, the reaction time is 24 hours.
4. The method for producing dihydromyrcenol as claimed in claim 1, wherein in the second step, the reaction temperature is 60 to 85 ℃.
5. The method for producing dihydromyrcenol as claimed in claim 4, wherein in the second step, the reaction temperature is 80 to 82 ℃.
6. The method for producing dihydromyrcenol according to claim 1, wherein in the second step, the mass ratio of the dihydromyrcenol to the liquid acid is 1:2 or 1:1.8 or 1:1.5.
7. The method for preparing dihydromyrcenol according to claim 1, wherein in the second step, the emulsifier is polyethylene glycol 600 emulsifier, and the amount of the emulsifier is:
The mass ratio of the polyethylene glycol 600 emulsifier to the dihydromyrcene is as follows: polyethylene glycol 600 emulsifier: dihydromyrcene=0.02-0.005: 1 or 0.01-0.02:1 or 0.015-0.02:1;
The emulsifier is OP10 emulsifier, and the mass ratio of the emulsifier to the dihydromyrcene is OP10 emulsifier: dihydromyrcene=0.015-0.008: 1 or 0.01-0.015:1 or 0.008-0.0014:1;
the mass ratio of the octadecylamine polyoxyethylene ether to the dihydromyrcene is as follows: octadecylamine polyoxyethylene ether: dihydromyrcene=0.03-0.015: 1 or 0.03-0.02:1 or 0.02-0.015:1.
8. The method for producing dihydromyrcenol as claimed in claim 1, wherein in the second step, the liquid acid concentration comprises the concentrations of the respective aqueous solutions of the following different acids:
The concentration of the trifluoromethyl sulfonic acid is 15% -20%;
the concentration of the methylsulfonic acid is 50% -70%.
9. The method for producing dihydromyrcenol as claimed in claim 1, wherein the recovery treatment comprises separating an oil phase from a water phase by a centrifuge from the emulsion after the reaction, subjecting the oil phase to alkali washing, separating and purifying by rectification, and diluting the liquid acid with water to the target requirement.
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| 二氢月桂烯水合制备二氢月桂烯醇的研究进展;俞忠华;周作良;陶建华;;江西科学(05) * |
| 强化气液两相传质的研究进展;成弘,周明,余国琮;化学进展(04);第315-322页 * |
| 超声波辅助合成水合萜二醇的工艺条件研究;王琳琳,陈小鹏,韦小杰,祝远姣;林产化工通讯(01);第7-11页 * |
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