CN113789220A - Oil tea oil refining method - Google Patents
Oil tea oil refining method Download PDFInfo
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- CN113789220A CN113789220A CN202111242759.7A CN202111242759A CN113789220A CN 113789220 A CN113789220 A CN 113789220A CN 202111242759 A CN202111242759 A CN 202111242759A CN 113789220 A CN113789220 A CN 113789220A
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- 239000003921 oil Substances 0.000 title claims abstract description 60
- 239000010495 camellia oil Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000007670 refining Methods 0.000 title claims abstract description 24
- 235000019198 oils Nutrition 0.000 claims abstract description 59
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 17
- 238000011221 initial treatment Methods 0.000 claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 240000001548 Camellia japonica Species 0.000 claims description 31
- 235000018597 common camellia Nutrition 0.000 claims description 31
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 26
- 229910021641 deionized water Inorganic materials 0.000 claims description 26
- 239000010779 crude oil Substances 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 22
- 238000007792 addition Methods 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 239000003607 modifier Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 241001122767 Theaceae Species 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229940074391 gallic acid Drugs 0.000 claims description 7
- 235000004515 gallic acid Nutrition 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims description 6
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 6
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 4
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000391 magnesium silicate Substances 0.000 abstract description 3
- 229910052919 magnesium silicate Inorganic materials 0.000 abstract description 3
- 235000019792 magnesium silicate Nutrition 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- 235000015112 vegetable and seed oil Nutrition 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000021588 free fatty acids Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- 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
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- 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
- C11B5/00—Preserving by using additives, e.g. anti-oxidants
- C11B5/0021—Preserving by using additives, e.g. anti-oxidants containing oxygen
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a method for refining oil tea oil, which belongs to the technical field of oil processing and comprises the following steps: mixing the oil tea seed oil subjected to primary treatment with an adsorption material at 105 ℃, stirring for 30min, and controlling the vacuum pressure at-0.06 MPa, and then filtering to obtain refined oil tea oil; the adsorption material is added in the camellia oil refining method, belongs to a magnesium silicate material, and is different from the existing material in that the raw material for preparing the adsorption material is modified nano silicon dioxide, so that the stability in the camellia oil refining process is improved, the stability of effective components in the camellia oil is improved, the acid value of the camellia oil is effectively reduced, the oxidation resistance of the camellia oil is improved, and the oil quality is ensured.
Description
Technical Field
The invention belongs to the technical field of oil processing, and particularly relates to a method for refining oil tea oil.
Background
The refining process of the oil tea oil has great influence on the quality of the oil tea oil, and the traditional refining process needs degumming, deacidification, decoloration, deodorization, dewaxing and the like. Degumming to remove colloid and impurities in oil; deacidifying is to neutralize free fatty acid in the grease with alkali; the decolorization is to remove pigments and trace metals in the grease, residual gum such as trace soap particles, phospholipid and the like and some substances with odor; deodorizing by steam distillation at high temperature and high vacuum, including foreign odor from the added auxiliary materials such as decolorizer; dewaxing is the removal of trace amounts of wax from oils and fats. Because the traditional refining process needs 5 working procedures, the process is complex and tedious, the refining consumption is high, auxiliary materials such as phosphoric acid, caustic soda flakes, activated clay and activated carbon are added, a large amount of loss of active ingredients such as vitamin e, tea polyphenol, squalene and sterol in the camellia seed oil is easily caused in long-time and high-strength (high-alkalinity substances such as caustic soda flakes participate in the reaction) treatment, the quality of the finished oil is seriously influenced, the risk of external hazards in the tea oil is increased due to the addition of various auxiliary materials, and the quality of the finished oil is reduced.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a method for refining oil tea oil.
The purpose of the invention can be realized by the following technical scheme:
a method for refining oil tea, which comprises the following steps:
mixing the oil tea seed oil subjected to primary treatment with an adsorption material, stirring at 105 deg.C for 30min under vacuum pressure of-0.06 MPa, and filtering to obtain refined oil tea oil;
further, the dosage-mass ratio of the oil-tea camellia seed oil subjected to primary treatment to the adsorbing material is 1000: 3.1-3.5.
The adsorbing material is prepared by the following steps:
mixing the modified nano silicon dioxide with deionized water, and performing ultrasonic dispersion for 1min under the condition that the ultrasonic frequency is 45kHz to obtain a first dispersion liquid;
mixing magnesium chloride hexahydrate, ammonium chloride and deionized water, stirring for 10min, and then adding ammonia water to obtain a second dispersion liquid;
and mixing and stirring the first dispersion liquid and the second dispersion liquid for 5min at the temperature of 20 ℃, then reacting for 12h at the temperature of 190 ℃, filtering after the reaction is finished, washing a filter cake with distilled water, and finally drying to constant weight at the temperature of 80 ℃ to obtain the adsorbing material.
Further, the dosage ratio of the modified nano silicon dioxide to the deionized water in the first dispersion liquid is 1 g: 12 mL; the dosage ratio of the magnesium chloride hexahydrate, the ammonium chloride, the deionized water and the ammonia water in the second dispersion liquid is 12.5 g: 5 g: 60mL of: 3mL, wherein the mass fraction of ammonia water is 40%; the volume ratio of the first dispersion to the second dispersion is 1: 1;
the modified nano-silica is prepared by the following steps:
step S11, modification by coupling agent: ultrasonically dispersing nano silicon dioxide and absolute ethyl alcohol in 40kHz frequency for 20min to obtain a suspension, mixing the absolute ethyl alcohol with deionized water, adjusting the pH value to 5 by using glacial acetic acid, then adding 3-aminopropyltrimethoxysilane, stirring for 10min, adding the suspension, stirring and reacting for 24h at the temperature of 25 ℃, then centrifuging the reaction solution, cleaning and centrifuging by using the absolute ethyl alcohol, the absolute tetrahydrofuran and acetone after centrifuging, dispersing the solid by using the deionized water, and freeze-drying to obtain a solid a; modifying the nano silicon dioxide by using a coupling agent to introduce amino;
step S12, mixing triacetyl gallic acid and chloroform, adding thionyl chloride while stirring at 40 ℃, keeping the temperature constant, continuously stirring for reaction for 5 hours, and after the reaction is finished, carrying out reduced pressure concentration to remove the solvent to obtain a modifier; performing chlorination modification on triacetyl gallic acid serving as an antioxidant component to obtain a modifier;
and step S13, adding the solid a and potassium carbonate into deionized water, adding a toluene solution of a modifier at the temperature of 0 ℃, heating to 25 ℃ after the addition is finished, reacting for 24 hours, performing vacuum filtration after the reaction is finished, washing with distilled water, and drying to constant weight under the vacuum condition of 50 ℃ after the washing is finished to obtain the modified nano-silica. The obtained solid a is prepared by reacting with a modifier, so that the nano silicon dioxide is modified, the stability of the modifier under the high-temperature condition is improved, and the nano silicon dioxide can be used as a raw material for preparing an adsorption material.
Further, in step S11, the ratio of the nano-silica to the absolute ethyl alcohol in the suspension is 3.5 g: 175 mL; the dosage ratio of the absolute ethyl alcohol, the deionized water, the 3-aminopropyl trimethoxy silane and the suspension is 160 mL: 20mL of: 7 g: 160 mL;
in the step S12, the dosage ratio of the triacetyl gallic acid to the chloroform to the thionyl chloride is 5 g: 50mL of: 12 mL;
in the step S13, the dosage ratio of the solid a, the potassium carbonate, the deionized water and the modifier is 5 g: 2 g: 40mL of: 2g of the total weight of the mixture; the toluene solution of the modifier is the modifier and toluene according to the dosage ratio of 1 g: 10mL of the above-mentioned components were mixed.
Further, the primary treatment process is as follows:
mixing the filtered and impurity-removed camellia seed crude oil with 85% of phosphoric acid by mass, wherein the addition amount of the phosphoric acid is 0.12-0.15% of the total weight of the camellia seed crude oil, reacting for 80-100min, heating to 50-60 ℃, adding a sodium hydroxide solution with Baume degree of 15, fully and uniformly mixing, and slowly stirring for about 20min to obtain mixed oil; the addition amount of the sodium hydroxide solution is as follows: 1 multiplied by 0.713 multiplied by Q/1000, wherein Q is the flow T/h of the crude oil of the camellia seeds; centrifugally separating the mixed oil, and separating soapstock in the mixed oil to obtain soapstock-removed oil; adding the desquamated oil into citric acid with the mass fraction of 50% and hot water with the temperature of 90 ℃, fully mixing, and then putting into a washing centrifuge for dehydration. The addition amount of citric acid is 0.01% of the total weight of the camellia seed crude oil, and the addition amount of hot water is 8% of the total weight of the camellia seed crude oil.
The invention has the beneficial effects that:
the adsorption material is added in the camellia oil refining method, belongs to a magnesium silicate material, and is different from the existing material in that the raw material for preparing the adsorption material is modified nano silicon dioxide, so that the stability in the camellia oil refining process is improved, the stability of effective components in the camellia oil is improved, the acid value of the camellia oil is effectively reduced, the oxidation resistance of the camellia oil is improved, and the oil quality is ensured.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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
Preparing modified nano silicon dioxide:
step S11, modification by coupling agent: ultrasonically dispersing nano silicon dioxide and absolute ethyl alcohol in 40kHz frequency for 20min to obtain a suspension, mixing the absolute ethyl alcohol with deionized water, adjusting the pH value to 5 by using glacial acetic acid, then adding 3-aminopropyltrimethoxysilane, stirring for 10min, adding the suspension, stirring and reacting for 24h at the temperature of 25 ℃, then centrifuging the reaction solution, cleaning and centrifuging by using the absolute ethyl alcohol, the absolute tetrahydrofuran and acetone after centrifuging, dispersing the solid by using the deionized water, and freeze-drying to obtain a solid a; wherein the dosage ratio of the nano silicon dioxide to the absolute ethyl alcohol in the suspension is 3.5 g: 175 mL; the dosage ratio of the absolute ethyl alcohol, the deionized water, the 3-aminopropyl trimethoxy silane and the suspension is 160 mL: 20mL of: 7 g: 160 mL;
step S12, mixing triacetyl gallic acid and chloroform, adding thionyl chloride while stirring at 40 ℃, keeping the temperature constant, continuously stirring for reaction for 5 hours, and after the reaction is finished, carrying out reduced pressure concentration to remove the solvent to obtain a modifier; wherein the dosage ratio of the triacetyl gallic acid to the chloroform to the thionyl chloride is 5 g: 50mL of: 12 mL;
and step S13, adding the solid a and potassium carbonate into deionized water, adding a toluene solution of a modifier at the temperature of 0 ℃, heating to 25 ℃ after the addition is finished, reacting for 24 hours, performing vacuum filtration after the reaction is finished, washing with distilled water, and drying to constant weight under the vacuum condition of 50 ℃ after the washing is finished to obtain the modified nano-silica. Wherein the dosage ratio of the solid a, the potassium carbonate, the deionized water and the modifier is 5 g: 2 g: 40mL of: 2g of the total weight of the mixture; the toluene solution of the modifier is the modifier and toluene according to the dosage ratio of 1 g: 10mL of the above-mentioned components were mixed.
Example 2
Preparing an adsorbing material:
mixing the modified nano silicon dioxide with deionized water, and performing ultrasonic dispersion for 1min under the condition that the ultrasonic frequency is 45kHz to obtain a first dispersion liquid; wherein the dosage ratio of the modified nano silicon dioxide to the deionized water is 1 g: 12 mL;
mixing magnesium chloride hexahydrate, ammonium chloride and deionized water, stirring for 10min, and then adding ammonia water to obtain a second dispersion liquid; wherein the dosage ratio of the magnesium chloride hexahydrate, the ammonium chloride, the deionized water and the ammonia water is 12.5 g: 5 g: 60mL of: 3mL, wherein the mass fraction of ammonia water is 40%;
and mixing and stirring the first dispersion liquid and the second dispersion liquid for 5min at the temperature of 20 ℃, then reacting for 12h at the temperature of 190 ℃, filtering after the reaction is finished, washing a filter cake with distilled water, and finally drying to constant weight at the temperature of 80 ℃ to obtain the adsorbing material. Wherein the volume ratio of the dosage of the first dispersion liquid to the dosage of the second dispersion liquid is 1: 1;
example 3
A method for refining oil tea, which comprises the following steps:
mixing the oil tea seed oil subjected to primary treatment with an adsorption material, stirring at 105 deg.C for 30min under vacuum pressure of-0.06 MPa, and filtering to obtain refined oil tea oil;
wherein the dosage mass ratio of the oil-tea camellia seed oil subjected to primary treatment to the adsorption material is 1000: 3.1. the adsorbent material was prepared as in example 2.
Primary treatment of camellia seed crude oil:
mixing the filtered and impurity-removed camellia seed crude oil with 85% phosphoric acid by mass, wherein the addition amount of the phosphoric acid is 0.12% of the total weight of the camellia seed crude oil, reacting for 80min, heating to 50 ℃, adding a sodium hydroxide solution with Baume degree of 15, fully and uniformly mixing, and slowly stirring for about 20min to obtain mixed oil; the addition amount of the sodium hydroxide solution is as follows: 1 multiplied by 0.713 multiplied by Q/1000, wherein Q is the flow T/h of the crude oil of the camellia seeds; centrifugally separating the mixed oil, and separating soapstock in the mixed oil to obtain soapstock-removed oil; adding the desquamated oil into citric acid with the mass fraction of 50% and hot water with the temperature of 90 ℃, fully mixing, and then putting into a washing centrifuge for dehydration. The addition amount of citric acid is 0.01% of the total weight of the camellia seed crude oil, and the addition amount of hot water is 8% of the total weight of the camellia seed crude oil.
Example 4
A method for refining oil tea, which comprises the following steps:
mixing the oil tea seed oil subjected to primary treatment with an adsorption material, stirring at 105 deg.C for 30min under vacuum pressure of-0.06 MPa, and filtering to obtain refined oil tea oil;
wherein the dosage mass ratio of the oil-tea camellia seed oil subjected to primary treatment to the adsorption material is 1000: 3.3. the adsorbent material was prepared as in example 2.
Primary treatment of camellia seed crude oil:
mixing the filtered and impurity-removed camellia seed crude oil with 85% phosphoric acid by mass, wherein the addition amount of the phosphoric acid is 0.13% of the total weight of the camellia seed crude oil, reacting for 90min, heating to 55 ℃, adding a sodium hydroxide solution with Baume degree of 15, fully and uniformly mixing, and slowly stirring for about 20min to obtain mixed oil; the addition amount of the sodium hydroxide solution is as follows: 1 multiplied by 0.713 multiplied by Q/1000, wherein Q is the flow T/h of the crude oil of the camellia seeds; centrifugally separating the mixed oil, and separating soapstock in the mixed oil to obtain soapstock-removed oil; adding the desquamated oil into citric acid with the mass fraction of 50% and hot water with the temperature of 90 ℃, fully mixing, and then putting into a washing centrifuge for dehydration. The addition amount of citric acid is 0.01% of the total weight of the camellia seed crude oil, and the addition amount of hot water is 8% of the total weight of the camellia seed crude oil.
Example 5
A method for refining oil tea, which comprises the following steps:
mixing the oil tea seed oil subjected to primary treatment with an adsorption material, stirring at 105 deg.C for 30min under vacuum pressure of-0.06 MPa, and filtering to obtain refined oil tea oil;
wherein the dosage mass ratio of the oil-tea camellia seed oil subjected to primary treatment to the adsorption material is 1000: 3.5. the adsorbent material was prepared as in example 2.
Primary treatment of camellia seed crude oil:
mixing the filtered and impurity-removed camellia seed crude oil with 85% phosphoric acid by mass, wherein the addition amount of the phosphoric acid is 0.15% of the total weight of the camellia seed crude oil, reacting for 100min, heating to 60 ℃, adding a sodium hydroxide solution with Baume degree of 15, fully and uniformly mixing, and slowly stirring for about 20min to obtain mixed oil; the addition amount of the sodium hydroxide solution is as follows: 1 multiplied by 0.713 multiplied by Q/1000, wherein Q is the flow T/h of the crude oil of the camellia seeds; centrifugally separating the mixed oil, and separating soapstock in the mixed oil to obtain soapstock-removed oil; adding the desquamated oil into citric acid with the mass fraction of 50% and hot water with the temperature of 90 ℃, fully mixing, and then putting into a washing centrifuge for dehydration. The addition amount of citric acid is 0.01% of the total weight of the camellia seed crude oil, and the addition amount of hot water is 8% of the total weight of the camellia seed crude oil.
Comparative example 1
The adsorbent material of example 4 was replaced with magnesium silicate and the rest of the process was kept unchanged.
The test results of the camellia oil obtained in examples 3 to 5 and comparative example 1 are shown in table 1 below:
TABLE 1
| Acid value (KOHmg/g) | Peroxide number (mmol/kg) | |
| Example 3 | 0.34 | 1.14 |
| Example 4 | 0.34 | 1.13 |
| Example 5 | 0.35 | 1.14 |
| Comparative example 1 | 1.22 | 2.51 |
From the above table 1, it can be seen that the refining method of the present invention can effectively reduce the acid value of the camellia seed oil and improve the oxidation resistance of the camellia seed oil.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. A method for refining oil tea oil is characterized by comprising the following steps: mixing the oil tea seed oil subjected to primary treatment with an adsorption material at 105 ℃, stirring for 30min, and controlling the vacuum pressure at-0.06 MPa, and then filtering to obtain refined oil tea oil;
the adsorbing material is prepared by the following steps:
mixing the modified nano silicon dioxide with deionized water, and performing ultrasonic dispersion for 1min to obtain a first dispersion liquid; mixing magnesium chloride hexahydrate, ammonium chloride and deionized water, stirring for 10min, and then adding ammonia water to obtain a second dispersion liquid; and mixing and stirring the first dispersion liquid and the second dispersion liquid for 5min at the temperature of 20 ℃, then reacting for 12h at the temperature of 190 ℃, filtering, washing and drying to constant weight after the reaction is finished, thus obtaining the adsorbing material.
2. The camellia oil refining method according to claim 1, wherein the dosage-mass ratio of the camellia oil subjected to primary treatment to the adsorbing material is 1000: 3.1-3.5.
3. The method for refining the oil tea camellia oil according to claim 1, wherein the amount ratio of the modified nano silica to the deionized water in the first dispersion is 1 g: 12 mL; the dosage ratio of the magnesium chloride hexahydrate, the ammonium chloride, the deionized water and the ammonia water in the second dispersion liquid is 12.5 g: 5 g: 60mL of: 3mL, wherein the mass fraction of ammonia water is 40%; the volume ratio of the first dispersion to the second dispersion is 1: 1.
4. the oil tea camellia oil refining method according to claim 1, wherein the modified nano silica is prepared by the following steps:
s11, ultrasonically dispersing nano silicon dioxide and absolute ethyl alcohol in 40kHz frequency for 20min to obtain a suspension, mixing the absolute ethyl alcohol and deionized water, adjusting the pH value to 5 by using glacial acetic acid, then adding 3-aminopropyltrimethoxysilane, stirring for 10min, adding the suspension, and stirring and reacting for 24h at 25 ℃ to obtain a solid a;
step S12, mixing triacetyl gallic acid and chloroform, adding thionyl chloride while stirring at 40 ℃, keeping the temperature unchanged, and continuously stirring for reaction for 5 hours to obtain a modifier;
and step S13, adding the solid a and potassium carbonate into deionized water, adding a toluene solution of a modifier at the temperature of 0 ℃, heating to 25 ℃ after the addition, and reacting for 24 hours to obtain the modified nano silicon dioxide.
5. The method for refining the oil tea camellia oil according to claim 4, wherein the amount ratio of the nano silicon dioxide to the absolute ethyl alcohol in the suspension in the step S11 is 3.5 g: 175 mL; the dosage ratio of the absolute ethyl alcohol, the deionized water, the 3-aminopropyl trimethoxy silane and the suspension is 160 mL: 20mL of: 7 g: 160 mL; in the step S12, the dosage ratio of the triacetyl gallic acid to the chloroform to the thionyl chloride is 5 g: 50mL of: 12 mL; in the step S13, the dosage ratio of the solid a, the potassium carbonate, the deionized water and the modifier is 5 g: 2 g: 40mL of: 2g of the total weight of the mixture; the toluene solution of the modifier is the modifier and toluene according to the dosage ratio of 1 g: 10mL of the above-mentioned components were mixed.
6. The method for refining the oil tea camellia oil according to claim 1, wherein the primary treatment process is as follows:
mixing the filtered and impurity-removed crude oil of the camellia seeds with phosphoric acid with the mass fraction of 85%, reacting for 80-100min, heating to 50-60 ℃, adding a sodium hydroxide solution with the Baume degree of 15, uniformly mixing, and stirring for 20min to obtain mixed oil; centrifugally separating the mixed oil, and separating soapstock in the mixed oil to obtain soapstock-removed oil; adding the desquamated oil into citric acid with the mass fraction of 50% and hot water with the temperature of 90 ℃, mixing, and then centrifugally dewatering.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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-
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Non-Patent Citations (3)
| Title |
|---|
| 于珊珊;李伯健;丁红;李金珠;李丹丹;: "经颅彩色多普勒超声在急性甲苯、二甲苯中毒诊断中的应用研究", 中国医疗设备, vol. 34, no. 12, pages 61 - 63 * |
| 张亚兰;俞政;: "甲基三烷基氯化铵的毒理学实验研究", 苏州大学学报(医学版), no. 1, pages 26 - 28 * |
| 陈雪帆;许配玉;陈爽;: "GC-MS法测定兰索拉唑原料中基因毒性杂质二氯亚砜", 中国药师, vol. 23, no. 07, pages 1461 - 1463 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117344398A (en) * | 2023-12-04 | 2024-01-05 | 潍坊瑞银纺织科技有限公司 | Large biological nylon fiber containing plant active ingredients and preparation method thereof |
| CN117344398B (en) * | 2023-12-04 | 2024-03-19 | 潍坊瑞银纺织科技有限公司 | Large biological nylon fiber containing plant active ingredients and preparation method thereof |
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