CN113201400A - Production process for preparing spice by extraction method - Google Patents
Production process for preparing spice by extraction method Download PDFInfo
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- CN113201400A CN113201400A CN202110434969.XA CN202110434969A CN113201400A CN 113201400 A CN113201400 A CN 113201400A CN 202110434969 A CN202110434969 A CN 202110434969A CN 113201400 A CN113201400 A CN 113201400A
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- sodium dichromate
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 235000013599 spices Nutrition 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 title claims abstract description 20
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000000463 material Substances 0.000 claims abstract description 35
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003513 alkali Substances 0.000 claims abstract description 24
- ZMQAAUBTXCXRIC-UHFFFAOYSA-N safrole Chemical compound C=CCC1=CC=C2OCOC2=C1 ZMQAAUBTXCXRIC-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 18
- VHVOLFRBFDOUSH-NSCUHMNNSA-N Isosafrole Chemical compound C\C=C\C1=CC=C2OCOC2=C1 VHVOLFRBFDOUSH-NSCUHMNNSA-N 0.000 claims abstract description 14
- VHVOLFRBFDOUSH-UHFFFAOYSA-N Isosafrole Natural products CC=CC1=CC=C2OCOC2=C1 VHVOLFRBFDOUSH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229950000244 sulfanilic acid Drugs 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000004821 distillation Methods 0.000 claims abstract description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 17
- 239000012043 crude product Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 13
- 239000013078 crystal Substances 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 239000012527 feed solution Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005194 fractionation Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 abstract description 8
- 230000008025 crystallization Effects 0.000 abstract description 8
- 239000002304 perfume Substances 0.000 abstract description 7
- 239000003205 fragrance Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000010692 aromatic oil Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 6
- 239000003921 oil Substances 0.000 description 4
- 235000019198 oils Nutrition 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000001640 fractional crystallisation Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- SATCULPHIDQDRE-UHFFFAOYSA-N piperonal Chemical compound O=CC1=CC=C2OCOC2=C1 SATCULPHIDQDRE-UHFFFAOYSA-N 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000008159 sesame oil Substances 0.000 description 1
- 235000011803 sesame oil Nutrition 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0007—Aliphatic compounds
- C11B9/0011—Aliphatic compounds containing S
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
Abstract
The invention discloses a production process for preparing spice by an extraction method, which comprises the following steps: the method comprises the following steps: preparing materials: the material comprises safrole, potassium hydroxide solution, alkali liquor, sulfanilic acid, sulfuric acid, sodium dichromate, benzene, ethanol and saturated saline; step two: adding safrole into a steamer, adding a potassium hydroxide solution into the steamer, heating, cooling, removing alkali liquor, and distilling to obtain isosafrole; step three: adding isosafrole into a reaction kettle, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, stirring to uniformly mix the materials, dropwise adding a sulfuric acid solution, heating to 55-60 ℃ by utilizing the reaction after dropwise adding is finished, keeping the temperature for 30-40min under stirring, and then cooling; the invention has the beneficial effects that: the preparation process is simplified, and the efficiency of spice production and processing is improved; the prepared perfume has purer fragrance by extraction, washing, distillation and crystallization.
Description
Technical Field
The invention belongs to the technical field of spice production, and particularly relates to a production process for preparing spices by an extraction method.
Background
The method for extracting the spice from the plant is various, and the common methods comprise three methods, namely a squeezing method, a distillation method and a leaching method. And (3) squeezing: the squeezing method is a general oil-making method, i.e. a method for squeezing the skin or fruit of the plant with strong pressure to make the oil flow out, such as directly taking the seed to squeeze (cold pressing method) to obtain the good but less flavor; if the seeds are heated (steamed or fried) and then pressed (hot pressing method), the obtained oil has low quality and large amount, and a screw press is preferably adopted for small-scale production; a distillation method: the method can be used for extracting the spices contained in barks, trunks or stems and leaves and the flowery odour which is not changed when being heated, but the method is not suitable for extracting the water-soluble spices, steam is firstly heated by opening steam to heat the pipe steam, the steam is then heated by opening the pipe when the water in a distiller boils, the steam enters an implant material layer in a metal mesh basket through a porous partition plate to carry out volatile oil component, the volatile oil component enters a condenser to be condensed into liquid once and flows into a liquid-water separator, the aromatic oil floats on the upper layer and then flows into a receiver, and the distillation process is carried out until no oil drops exist in condensed flow liquid; if some aromatic oil is not easy to be brought out with water vapor at 100 ℃, the water in the distiller can be changed into saturated salt water to increase the boiling temperature so as to bring out the aromatic oil; if necessary, the aromatic oil extracted by the steam distillation method can be further processed, such as precise fractionation, solvent extraction, fractional crystallization; the leaching method comprises the following steps: the aromatic oil can be dissolved in most organic solvents, such as alcohol, ether, and petroleum essence, and if the flower containing the aromatic oil is immersed in such solvents, the aromatic oil is transferred into the solvents, if the solvents are alcohol, the aromatic oil is obtained as perfume, and if the solvents are other solvents, the solvents can be heated at low temperature to evaporate, and the aromatic oil remains; the sesame oil obtained by this method usually contains plant alkaloid and fat.
With the improvement of living standard of people, only natural perfume is not enough, so people begin to research the method of organic synthesis to produce synthetic perfume with good quality, low price and large production capacity; the heliotropin is white or light yellow crystal, has the fragrance of sweet bean and anisyl, has the boiling point of 263 ℃ and the melting point of 37 ℃, is dissolved in ethanol and oil, is insoluble in glycerin and water, is easy to change color when being exposed to light and heat, is an important synthetic spice, and is widely applied to cosmetics and edible essence.
In order to improve the efficiency of perfume production and processing and ensure pure fragrance, a production process beneficial to an extraction method for preparing perfume is provided.
Disclosure of Invention
The invention aims to provide a production process for preparing spices by an extraction method, which is beneficial to improving the efficiency of spice production and processing and ensuring pure fragrance.
In order to achieve the purpose, the invention provides the following technical scheme: a production process for preparing spices by using an extraction method is as follows:
the method comprises the following steps: preparing materials: the material comprises safrole, potassium hydroxide solution, alkali liquor, sulfanilic acid, sulfuric acid, sodium dichromate, benzene, ethanol and saturated saline;
step two: adding safrole into a steamer, adding a potassium hydroxide solution into the steamer, heating, cooling, removing alkali liquor, and distilling to obtain isosafrole;
step three: adding isosafrole into a reaction kettle, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, stirring to uniformly mix the materials, dropwise adding a sulfuric acid solution, heating to 55-60 ℃ by utilizing the reaction after dropwise adding is finished, keeping the temperature for 30-40min under stirring, and then cooling;
step four: cooling the materials, pouring the materials into a separating funnel, adding benzene for extraction, shaking, adding an equal amount of warm water into the extract liquid for washing, then adding alkali liquor and adjusting the pH value to be neutral, then washing with sodium carbonate solution, and finally washing with saturated saline water;
step five: adding the benzene extracting solution into a distillation flask, heating to recover benzene, and then carrying out vacuum fractionation to obtain a crude product;
step six: pouring the crude product into a crystallizing tray while the crude product is hot, naturally crystallizing, then placing into a refrigerator, standing overnight, breaking the frozen hard crystal, washing with ethanol at normal temperature, filtering, centrifuging, heating to melt the crystal, freezing for crystallizing, and finally drying in a blast drying oven.
As a preferable technical scheme of the invention, the alkali liquor is sodium hydroxide solution.
As a preferred technical solution of the present invention, the preparation method of the sodium dichromate comprises the following steps:
the method comprises the following steps: mixing an industrial sodium chromate solution and a sodium dichromate solution with a concentration of sodium dichromate to prepare an anode mixed feed solution, and introducing the anode mixed feed solution into an anode chamber;
step two: mixing a sodium hydroxide solution and pure water to prepare a cathode mixed feed liquid, and introducing the cathode mixed feed liquid into a cathode chamber;
step three: and D, connecting direct current to carry out electrolytic reaction, and obtaining sodium dichromate in the anode chamber after the electrolytic reaction.
As a preferable technical scheme of the invention, in the second step, the temperature is raised to 140-160 ℃, the alkali liquor is cooled and discarded, and the isosafrole is obtained by distillation.
In the third step, sodium dichromate, water and sulfanilic acid are added into the reaction kettle, and the mixture is stirred for 5-15min at a speed of 50 r/min.
As a preferred technical scheme of the invention, in the fourth step, the temperature of the materials is reduced to 40 ℃, the materials are poured into a separating funnel, the benzene is added for extraction, and the materials are shaken for 3-5 min.
In the sixth step, the container is placed in a refrigerator and kept at the temperature of minus 5-18 ℃ overnight.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation process is simplified, and the efficiency of spice production and processing is improved;
(2) the prepared perfume has purer fragrance by extraction, washing, distillation and crystallization.
Drawings
FIG. 1 is a flow chart of the production process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, the present invention provides a technical solution: a production process for preparing spice by an extraction method is as follows:
the method comprises the following steps: preparing materials: the material comprises safrole, potassium hydroxide solution, alkali liquor, sulfanilic acid, sulfuric acid, sodium dichromate, benzene, ethanol and saturated saline;
step two: adding safrole into a steamer, adding a potassium hydroxide solution into the steamer, heating to 150 ℃, cooling, removing alkali liquor, and distilling to obtain isosafrole;
step three: adding isosafrole into a reaction kettle, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, stirring at 50r/min for 10min to uniformly mix the materials, dropwise adding a sulfuric acid solution, heating to 58 ℃ by using a reaction after dropwise adding, keeping the temperature for 35min under stirring, and cooling;
step four: cooling the materials to 40 ℃, pouring the materials into a separating funnel, adding benzene for extraction, shaking for 4min, adding an equal amount of warm water into the extract liquid for washing, then adding alkali liquor and adjusting the pH value to be neutral, then washing with a sodium carbonate solution, and finally washing with saturated saline;
step five: adding the benzene extracting solution into a distillation flask, heating to recover benzene, and then carrying out vacuum fractionation to obtain a crude product;
step six: pouring the crude product into a crystallization tray while the crude product is hot, naturally crystallizing, then placing into a refrigerator, overnight at-12 ℃, breaking frozen hard crystals, cleaning with ethanol at normal temperature, filtering, spin-drying with a centrifuge, heating to melt the crystals, freezing for crystallization, and finally drying in a blast drying oven.
In this embodiment, the alkali solution is preferably sodium hydroxide solution.
In this embodiment, the preferred preparation method of sodium dichromate is as follows:
the method comprises the following steps: mixing an industrial sodium chromate solution and a sodium dichromate solution with a concentration of sodium dichromate to prepare an anode mixed feed solution, and introducing the anode mixed feed solution into an anode chamber;
step two: mixing a sodium hydroxide solution and pure water to prepare a cathode mixed feed liquid, and introducing the cathode mixed feed liquid into a cathode chamber;
step three: and D, connecting direct current to carry out electrolytic reaction, and obtaining sodium dichromate in the anode chamber after the electrolytic reaction.
Example 2
Referring to fig. 1, the present invention provides a technical solution: a production process for preparing spice by an extraction method is as follows:
the method comprises the following steps: preparing materials: the material comprises safrole, potassium hydroxide solution, alkali liquor, sulfanilic acid, sulfuric acid, sodium dichromate, benzene, ethanol and saturated saline;
step two: adding safrole into a steamer, adding a potassium hydroxide solution into the steamer, heating to 140 ℃, cooling, removing alkali liquor, and distilling to obtain isosafrole;
step three: adding isosafrole into a reaction kettle, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, stirring at 50r/min for 5min to uniformly mix the materials, dropwise adding a sulfuric acid solution, heating to 55 ℃ by using a reaction after dropwise adding, keeping the temperature for 30min under stirring, and cooling;
step four: cooling the materials to 40 ℃, pouring the materials into a separating funnel, adding benzene for extraction, shaking for 3min, adding an equal amount of warm water into the extract liquid for washing, then adding alkali liquor and adjusting the pH value to be neutral, then washing with a sodium carbonate solution, and finally washing with saturated saline;
step five: adding the benzene extracting solution into a distillation flask, heating to recover benzene, and then carrying out vacuum fractionation to obtain a crude product;
step six: pouring the crude product into a crystallization tray while the crude product is hot, naturally crystallizing, then placing into a refrigerator, overnight at-5 ℃, breaking frozen hard crystals, cleaning with ethanol at normal temperature, filtering, spin-drying with a centrifuge, heating to melt the crystals, freezing for crystallization, and finally drying in a blast drying oven.
In this embodiment, the alkali solution is preferably sodium hydroxide solution.
In this embodiment, the preferred preparation method of sodium dichromate is as follows:
the method comprises the following steps: mixing an industrial sodium chromate solution and a sodium dichromate solution with a concentration of sodium dichromate to prepare an anode mixed feed solution, and introducing the anode mixed feed solution into an anode chamber;
step two: mixing a sodium hydroxide solution and pure water to prepare a cathode mixed feed liquid, and introducing the cathode mixed feed liquid into a cathode chamber;
step three: and D, connecting direct current to carry out electrolytic reaction, and obtaining sodium dichromate in the anode chamber after the electrolytic reaction.
Example 3
Referring to fig. 1, the present invention provides a technical solution: a production process for preparing spice by an extraction method is as follows:
the method comprises the following steps: preparing materials: the material comprises safrole, potassium hydroxide solution, alkali liquor, sulfanilic acid, sulfuric acid, sodium dichromate, benzene, ethanol and saturated saline;
step two: adding safrole into a steamer, adding a potassium hydroxide solution into the steamer, heating to 160 ℃, cooling, removing alkali liquor, and distilling to obtain isosafrole;
step three: adding isosafrole into a reaction kettle, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, stirring at 50r/min for 15min to uniformly mix the materials, dropwise adding a sulfuric acid solution, heating to 60 ℃ by using a reaction after dropwise adding, keeping the temperature for 40min under stirring, and cooling;
step four: cooling the materials to 40 ℃, pouring the materials into a separating funnel, adding benzene for extraction, shaking for 5min, adding the same amount of warm water into the extract liquid for washing, then adding alkali liquor and adjusting the pH value to be neutral, then washing with sodium carbonate solution, and finally washing with saturated saline water;
step five: adding the benzene extracting solution into a distillation flask, heating to recover benzene, and then carrying out vacuum fractionation to obtain a crude product;
step six: pouring the crude product into a crystallization tray while the crude product is hot, naturally crystallizing, then placing into a refrigerator, overnight at-18 ℃, breaking frozen hard crystals, cleaning with ethanol at normal temperature, filtering, spin-drying with a centrifuge, heating to melt the crystals, freezing for crystallization, and finally drying in a blast drying oven.
In this embodiment, the alkali solution is preferably sodium hydroxide solution.
In this embodiment, the preferred preparation method of sodium dichromate is as follows:
the method comprises the following steps: mixing an industrial sodium chromate solution and a sodium dichromate solution with a concentration of sodium dichromate to prepare an anode mixed feed solution, and introducing the anode mixed feed solution into an anode chamber;
step two: mixing a sodium hydroxide solution and pure water to prepare a cathode mixed feed liquid, and introducing the cathode mixed feed liquid into a cathode chamber;
step three: and D, connecting direct current to carry out electrolytic reaction, and obtaining sodium dichromate in the anode chamber after the electrolytic reaction.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A production process for preparing spices by using an extraction method is characterized by comprising the following steps: the production process comprises the following steps:
the method comprises the following steps: preparing materials: the material comprises safrole, potassium hydroxide solution, alkali liquor, sulfanilic acid, sulfuric acid, sodium dichromate, benzene, ethanol and saturated saline;
step two: adding safrole into a steamer, adding a potassium hydroxide solution into the steamer, heating, cooling, removing alkali liquor, and distilling to obtain isosafrole;
step three: adding isosafrole into a reaction kettle, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, stirring to uniformly mix the materials, dropwise adding a sulfuric acid solution, heating to 55-60 ℃ by utilizing the reaction after dropwise adding is finished, keeping the temperature for 30-40min under stirring, and then cooling;
step four: cooling the materials, pouring the materials into a separating funnel, adding benzene for extraction, shaking, adding an equal amount of warm water into the extract liquid for washing, then adding alkali liquor and adjusting the pH value to be neutral, then washing with sodium carbonate solution, and finally washing with saturated saline water;
step five: adding the benzene extracting solution into a distillation flask, heating to recover benzene, and then carrying out vacuum fractionation to obtain a crude product;
step six: pouring the crude product into a crystallizing tray while the crude product is hot, naturally crystallizing, then placing into a refrigerator, standing overnight, breaking the frozen hard crystal, washing with ethanol at normal temperature, filtering, centrifuging, heating to melt the crystal, freezing for crystallizing, and finally drying in a blast drying oven.
2. The extraction-facilitated production process for making a spice according to claim 1, wherein: the alkali liquor is sodium hydroxide solution.
3. The extraction-facilitated production process for making a spice according to claim 1, wherein: the preparation method of the sodium dichromate comprises the following steps:
the method comprises the following steps: mixing an industrial sodium chromate solution and a sodium dichromate solution with a concentration of sodium dichromate to prepare an anode mixed feed solution, and introducing the anode mixed feed solution into an anode chamber;
step two: mixing a sodium hydroxide solution and pure water to prepare a cathode mixed feed liquid, and introducing the cathode mixed feed liquid into a cathode chamber;
step three: and D, connecting direct current to carry out electrolytic reaction, and obtaining sodium dichromate in the anode chamber after the electrolytic reaction.
4. The extraction-facilitated production process for making a spice according to claim 1, wherein: in the second step, the temperature is raised to 140-160 ℃, cooling is carried out, alkali liquor is discarded, and the isosafrole is obtained by distillation.
5. The extraction-facilitated production process for making a spice according to claim 1, wherein: and in the third step, adding sodium dichromate, water and sulfanilic acid into the reaction kettle, and stirring for 5-15min at the speed of 50 r/min.
6. The extraction-facilitated production process for making a spice according to claim 1, wherein: and in the fourth step, the temperature of the materials is reduced to 40 ℃, the materials are poured into a separating funnel, the benzene is added for extraction, and the materials are shaken for 3-5 min.
7. The extraction-facilitated production process for making a spice according to claim 1, wherein: and step six, putting the mixture into a refrigerator and standing overnight at the temperature of minus 5-18 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827695A (en) * | 2012-08-16 | 2012-12-19 | 吴江市曙光化工有限公司 | Production method of sassafras oil |
| CN104262320A (en) * | 2014-10-09 | 2015-01-07 | 广西壮族自治区林业科学研究院 | Method for converting safrole into iso-safrole |
-
2021
- 2021-04-22 CN CN202110434969.XA patent/CN113201400A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827695A (en) * | 2012-08-16 | 2012-12-19 | 吴江市曙光化工有限公司 | Production method of sassafras oil |
| CN104262320A (en) * | 2014-10-09 | 2015-01-07 | 广西壮族自治区林业科学研究院 | Method for converting safrole into iso-safrole |
Non-Patent Citations (3)
| Title |
|---|
| 唐健: "黄樟油素的开发与利用", 《河北化工》 * |
| 孙凌峰: "黄樟素的天然来源及其在合成香料中的利用", 《香料香精化妆品》 * |
| 罗小龙: "黄樟油素的生产及应用", 《林产化工通讯》 * |
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Application publication date: 20210803 |