CN106833888A - A kind of efficient method for acid stripping and refining of tea seed crude oil - Google Patents

A kind of efficient method for acid stripping and refining of tea seed crude oil Download PDF

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Publication number
CN106833888A
CN106833888A CN201710123680.XA CN201710123680A CN106833888A CN 106833888 A CN106833888 A CN 106833888A CN 201710123680 A CN201710123680 A CN 201710123680A CN 106833888 A CN106833888 A CN 106833888A
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China
Prior art keywords
crude oil
tea seed
seed crude
oil
refining
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Pending
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CN201710123680.XA
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Chinese (zh)
Inventor
袁传勋
周雷
金日生
刘国功
余光明
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Anhui Mountain Biotechnology Co Ltd
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Anhui Mountain Biotechnology Co Ltd
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Priority to CN201710123680.XA priority Critical patent/CN106833888A/en
Publication of CN106833888A publication Critical patent/CN106833888A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter

Abstract

The invention discloses a kind of efficient method for acid stripping and refining of tea seed crude oil; small molecule alcohol can be preferably dissolved in using free fatty in tea seed crude oil; and neutral oil is the characteristics of be insoluble in small molecule alcohol; extraction depickling is carried out to tea seed crude oil using the mixed liquor of absolute ethyl alcohol and glycerine; glycerine is miscible in ethanol; increased its collision opportunity that aliphatic acid is extracted with ethanol; a part of aliphatic acid is set to generate triglycerides with glycerine reaction; oil product yield is improve, while to being filled with nitrogen in extraction flask to protect the nutritional ingredient in grease not oxidized.The inventive method had not only retained nutritional ingredient but also had improved oil product yield, meanwhile, also there is non-environmental-pollution, low energy consumption.

Description

A kind of efficient method for acid stripping and refining of tea seed crude oil
Technical field
The present invention relates to a kind of method of refining of edible oil and fat, and in particular to a kind of efficient acid stripping and refining side of tea seed crude oil Method.
Background technology
Tea oil is the distinctive xylophyta of China, aboundresources.Tea oil aliphatic acid is main by oleic acid, linoleic acid and a small amount of Saturated fatty acid is constituted, and has the laudatory title of " east olive oil ".Also contain several functions composition such as VE, sterol, spiny dogfish in tea oil Alkene etc..The refined camellia oil of domestic market supply is mainly using the method for alkali-refining deacidification.The method can significantly drop The acid value of low tea oil, but the effect of alkali can cause the multiple efficacies component damages in tea oil;Meanwhile, can be one under caustic refining conditions There is hydrolysis in amount of grease, reduce the yield of oil product.Therefore, invention one kind can effectively reduce tea oil acid value again can be with The new acid stripping method for improving oil and fat refining yield and to greatest extent retaining the nutritional ingredient in tea oil has great importance.
The content of the invention
The technical problems to be solved by the invention are:For the nutritional ingredient caused during alkali-refining deacidification in tea seed crude oil and A kind of loss of amount of grease, there is provided efficient method for acid stripping and refining of tea seed crude oil, this method ensure high yield pulp1 in the case of again The nutritional ingredient in crude oil can to greatest extent be retained.
For the technical solution adopted by the present invention that solves the above problems is as follows:
A kind of efficient method for acid stripping and refining of tea seed crude oil, it is characterised in that comprise the following steps:
(1) filter
Tea seed crude oil is filtered to its impurity content at normal temperatures and is less than 0.2wt%;
(2) degumming
The phosphoric acid of quality of crude oil 0.1-0.4% is added in tea seed crude oil after filtration, and is stirred under the conditions of 70-80 DEG C 20-25min, adds the same warm water of quality of crude oil 4-7% and stirs 30-40min, 2-4h is stood, then in 3500- 10-15min degummings are centrifuged under the conditions of 4500rpm;
(3) depickling
It is 1 by the mass ratio of crude oil and extractant by the crude oil after degumming:The ratio of 1-2 adds extractant, is protected in nitrogen Under shield, under the conditions of 30-40 DEG C, 25-35min is sufficiently mixed with the mixing speed of 60-80r/min, then by water phase and oil phase Point liquid, oil phase distillation removing extractant is obtained into depickling tea seed crude oil;
(4) decolourize
Tea seed crude oil after depickling is processed is heated to 80-90 DEG C, adds taking off for the tea seed quality of crude oil 1-2% after depickling Toner decolouring 20-30min,
(5) deodorization
Tea seed crude oil after decolouring processes 10-20min under the conditions of vacuum 3000-5000pa, 200-240 DEG C of temperature and takes off It is smelly;
(6) dewax
Tea seed crude oil after deodorization is cooled to 5-10 DEG C with the freezing rate of 0.8-1.2 DEG C/h, treats consolidating in tea seed crude oil Static pressure filtration treatment is carried out after body fat crystallization, refined tea oil is obtained.
Described a kind of efficient method for acid stripping and refining of tea seed crude oil, it is characterised in that the extractant described in step (3) is sweet Oil and absolute ethyl alcohol press 1:The mixed liquor that the volume ratio of 10-15 is obtained by mixing.
Described a kind of efficient method for acid stripping and refining of tea seed crude oil, it is characterised in that used in step (4) decolorization Decolorising agent is that activated carbon presses 1 with diatomite:The mixture being obtained by mixing of the mass ratio of 1.5-2.5.
The acid number of step (1) the tea seed crude oil is in 5-8mgKOH/g.
The present invention by acid number for the tea seed crude oil of 5-8mgKOH/g is processed into first-level tea oil, refining yield more than 93%, Oil yield about 6% or so is improved than alkali refining method.The nutrient composition content in refined tea oil is than alkali-refining process gained tea oil simultaneously Have greatly improved, wherein VE many 70%, sterol is more 8 times, squalene many 50%.Product quality meets national standard GB11765-2003 squeezes primary standard.
Specific embodiment
Embodiment 1
A kind of efficient method for acid stripping and refining of tea seed crude oil, comprises the following steps:
(1) filter
Acid number is taken to be filtered at normal temperatures to its impurity content less than 0.2wt% in the tea seed crude oil of 6-10mgKOH/g.
(2) degumming
The 0.2% of its quality phosphoric acid is added in tea seed crude oil after filtration, and 20min is stirred under the conditions of 75 DEG C, Add the 5% of quality of crude oil same warm water and stir 30min, stand 3h, 15min is then centrifuged under the conditions of 4000rpm Degumming;
(3) depickling
The free fatty in tea seed crude oil is isolated using the method for extraction, under the conditions of 35 DEG C, by crude oil and extraction Agent is 1:1 mass ratio adds extractant, under conditions of nitrogen is passed through, is sufficiently mixed with the mixing speed of 60r/min 30min.Oil phase distillation removing extractant is taken after point liquid and obtains depickling tea seed crude oil;
Wherein extractant is that glycerine and absolute ethyl alcohol press 1:The liquid that 12 volume ratio is obtained by mixing;
(4) decolourize
Tea seed crude oil after depickling is processed is heated to 80 DEG C, and the decolorising agent of tea seed quality of crude oil 1% takes off after addition depickling Color 25min;
Wherein decolorising agent is that activated carbon presses 1 with diatomite:The mixture being obtained by mixing of 1.5 mass ratio;
(5) deodorization
Tea seed crude oil after decolouring processes 15min deodorizations under the conditions of vacuum 4000pa, 220 DEG C of temperature;
(6) dewax
Tea seed crude oil after deodorization is cooled to 5 DEG C with the freezing rate of 1.0 DEG C/h, treats the solid fat crystallization in tea seed crude oil After carry out static pressure filtration treatment, obtain refined tea oil.
Embodiment 2
A kind of efficient method for acid stripping and refining of tea seed crude oil, comprises the following steps:
(1) filter
Acid number is taken to be filtered at normal temperatures to its impurity content less than 0.2wt% in the tea seed crude oil of 6-10mgKOH/g.
(2) degumming
The 0.3% of its quality phosphoric acid is added in tea seed crude oil after filtration, and 25min is stirred under the conditions of 80 DEG C, Add the 6% of quality of crude oil same warm water and stir 40min, stand 4h, 15min is then centrifuged under the conditions of 4000rpm Degumming;
(3) depickling
The free fatty in tea seed crude oil is isolated using the method for extraction, under the conditions of 40 DEG C, by crude oil and extraction Agent is 1:1.5 mass ratio adds extractant, under conditions of nitrogen is passed through, is sufficiently mixed with the mixing speed of 80r/min 35min.Oil phase distillation removing extractant is taken after point liquid and obtains depickling tea seed crude oil;
Wherein extractant is that glycerine and absolute ethyl alcohol press 1:The liquid of 12 volume ratio mixing;
(4) decolourize
Tea seed crude oil after depickling is processed is heated to 90 DEG C, adds the decolorising agent of tea seed quality of crude oil 1.5% after depickling Decolouring 30min;
Wherein decolorising agent is that activated carbon presses 1 with diatomite:The mixing decolorising agent of 2 mass ratio;
(5) deodorization
Tea seed crude oil after decolouring processes 20min deodorizations under the conditions of vacuum 4000pa, 240 DEG C of temperature;
(6) dewax
Tea seed crude oil after deodorization is cooled to 5 DEG C with the freezing rate of 1.0 DEG C/h, treats the solid fat crystallization in tea seed crude oil After carry out static pressure filtration treatment, obtain refined tea oil.
Comparative example 1
A kind of method of alkali-refining deacidification, comprises the following steps:
(1) filter
Acid number is taken to be filtered at normal temperatures to its impurity content less than 0.2wt% in the tea seed crude oil of 6-10mgKOH/g.
(2) degumming
The 0.2% of its quality phosphoric acid is added in tea seed crude oil after filtration, and 20min is stirred under the conditions of 75 DEG C, Add the 5% of quality of crude oil same warm water and stir 30min, stand 3h, 15min is then centrifuged under the conditions of 4000rpm Degumming.
(3) depickling
The free fatty in tea seed crude oil is removed using the method for alkali-refining deacidification.Tea seed crude oil after degumming is heated to 50 DEG C, the concentration for adding the 7.5% of tea seed quality of crude oil is the sodium hydroxide solution of 8wt%, stirs 20min, adds tea seed The water of 50 DEG C of the 15% of quality of crude oil, stands 4h, is removed water with sedimentation separation method and gleditsia sinensis.
(4) decolourize
Tea seed crude oil after depickling is processed is heated to 80 DEG C, and the decolorising agent of tea seed quality of crude oil 1% takes off after addition depickling Color 25min.
Wherein decolorising agent is that activated carbon presses 1 with diatomite:The mixing decolorising agent of 2 mass ratio.
(5) deodorization
Tea seed crude oil after decolouring processes 15min deodorizations under the conditions of vacuum 4000pa, 220 DEG C of temperature.
(6) dewax
Tea seed crude oil after deodorization is cooled to 5 DEG C with the freezing rate of 1.0 DEG C/h, treats the solid fat crystallization in tea seed crude oil After carry out static pressure filtration treatment, obtain refined tea oil.
Comparative example 2
A kind of method of preparing first-level tea oil by alcohol extraction and deacidification, comprises the following steps:
(1) filter
Acid number is taken to be filtered at normal temperatures to its impurity content less than 0.2wt% in the tea seed crude oil of 6-10mgKOH/g.
(2) degumming
20% water, 70 DEG C of hydration temperature, hydration time 20min are added in tea seed crude oil.
(3) it is vacuum dried
Tea seed crude oil after degumming is heated up into 100 DEG C carries out dewater treatment into vacuum desiccator, vacuum for- 0.092MPa, tea seed crude oil moisture is less than 0.8% after dehydration.
(4) depickling is extracted
Tea seed crude oil after vacuum drying is cooled to 45 DEG C, is then 1 by crude oil and alcohol ratio:1.5 ratio is added The alcohol of mass concentration 95% is mixed, and 20min is sufficiently stirred under 65r/min, and extraction temperature is controlled at 45 DEG C.
(5) decolourize
Tea seed crude oil after depickling is processed is heated to 90 DEG C, adds the decolorising agent of tea seed quality of crude oil 1.5% after depickling Decolouring 30min.
Wherein decolorising agent is that activated carbon presses 1 with diatomite:The mixing decolorising agent of 2 mass ratio.
(6) deodorization
Tea seed crude oil after decolouring processes 20min deodorizations under the conditions of vacuum 4000pa, 240 DEG C of temperature.
(7) dewax
Tea seed crude oil after deodorization is cooled to 5 DEG C with the freezing rate of 1.0 DEG C/h, treats the solid fat crystallization in tea seed crude oil After carry out static pressure filtration treatment, obtain refined tea oil.
The quality index and nutrient composition content of each embodiment gained refined oil are as shown in the table:
The present invention is used as can be seen from the above table process for purification and traditional alkali refining processing technology and a kind of alcoholic extract Take depickling and prepare the method for first-level tea oil compared to being improved to some extent on oil yield, product quality meets national standard GB11765-2003 squeezes primary standard.Meanwhile, the nutrition in it preferably can retain tea oil in the case of ensureing low acid value Composition such as VE, sterol and squalene etc..

Claims (4)

1. a kind of efficient method for acid stripping and refining of tea seed crude oil, it is characterised in that comprise the following steps:
(1)Filtering
Tea seed crude oil is filtered to its impurity content at normal temperatures and is less than 0.2wt%;
(2)Degumming
The phosphoric acid of quality of crude oil 0.1-0.4% is added in tea seed crude oil after filtration, and 20- is stirred under the conditions of 70-80 DEG C 25min, adds the same warm water of quality of crude oil 4-7% and stirs 30-40min, 2-4h is stood, then in 3500-4500rpm Under the conditions of be centrifuged 10-15min degummings;
(3)Depickling
It is 1 by the mass ratio of crude oil and extractant by the crude oil after degumming:The ratio of 1-2 adds extractant, in nitrogen protection Under, under the conditions of 30-40 DEG C, 25-35min is sufficiently mixed with the mixing speed of 60-80r/min, then by water phase and oil phase Divide liquid, oil phase distillation removing extractant is obtained into depickling tea seed crude oil;
(4)Decolourize
Tea seed crude oil after depickling is processed is heated to 80-90 DEG C, adds the decolorising agent of the tea seed quality of crude oil 1-2% after depickling Decolouring 20-30min,
(5)Deodorization
Tea seed crude oil after decolouring processes 10-20min deodorizations under the conditions of vacuum 3000-5000pa, 200-240 DEG C of temperature;
(6)Dewaxing
Tea seed crude oil after deodorization is cooled to 5-10 DEG C with the freezing rate of 0.8-1.2 DEG C/h, treats the solid fat in tea seed crude oil Static pressure filtration treatment is carried out after crystallization, refined tea oil is obtained.
2. a kind of efficient method for acid stripping and refining of tea seed crude oil according to claim 1, it is characterised in that step(3)It is described Extractant press 1 for glycerine and absolute ethyl alcohol:The mixed liquor that the volume ratio of 10-15 is obtained by mixing.
3. a kind of efficient method for acid stripping and refining of tea seed crude oil according to claim 1, it is characterised in that step(4)Decolourize During the decolorising agent that uses for activated carbon with diatomite by 1:The mixture being obtained by mixing of the mass ratio of 1.5-2.5.
4. a kind of efficient method for acid stripping and refining of tea seed crude oil according to claim 1, it is characterised in that:
Step(1)The acid number of the tea seed crude oil is in 5-8mgKOH/g.
CN201710123680.XA 2017-03-03 2017-03-03 A kind of efficient method for acid stripping and refining of tea seed crude oil Pending CN106833888A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108913343A (en) * 2018-08-06 2018-11-30 贵州布依仁农业科技有限公司 A kind of oil tea oil expression method
CN109181865A (en) * 2018-11-16 2019-01-11 华中农业大学 A kind of deodorization treatment process of edible oil
CN110951538A (en) * 2019-11-19 2020-04-03 山东华胜检验检测技术有限公司 Physical refining production process of peanut oil
CN111996076A (en) * 2020-09-10 2020-11-27 江西齐云山油茶科技有限公司 Process for reducing free fatty acid of camellia oil by using enzymatic esterification method
CN112831371A (en) * 2019-11-24 2021-05-25 湖南大三湘茶油股份有限公司 High-quality colorless tea oil and preparation method thereof
CN112831372A (en) * 2019-11-25 2021-05-25 湖南大三湘茶油股份有限公司 Pure camellia oil and preparation method thereof
CN112877133A (en) * 2021-01-05 2021-06-01 贵州乔盛生物科技有限公司 Tea oil extraction method

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Publication number Priority date Publication date Assignee Title
CN101717689A (en) * 2009-11-18 2010-06-02 广东新大地生物科技股份有限公司 Method for preparing first-level tea oil by alcohol extraction and deacidification
CN104232292A (en) * 2014-09-16 2014-12-24 锦屏县食为天农产品有限公司 Cold pressing and refining method of camellia oil
CN104862072A (en) * 2015-05-08 2015-08-26 湖南红星盛康油脂股份有限公司 Tea seed oil refining process
CN105132156A (en) * 2015-08-28 2015-12-09 成都市新津迎先粮油有限公司 Method for refining rape-seed raw oil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101717689A (en) * 2009-11-18 2010-06-02 广东新大地生物科技股份有限公司 Method for preparing first-level tea oil by alcohol extraction and deacidification
CN104232292A (en) * 2014-09-16 2014-12-24 锦屏县食为天农产品有限公司 Cold pressing and refining method of camellia oil
CN104862072A (en) * 2015-05-08 2015-08-26 湖南红星盛康油脂股份有限公司 Tea seed oil refining process
CN105132156A (en) * 2015-08-28 2015-12-09 成都市新津迎先粮油有限公司 Method for refining rape-seed raw oil

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108913343A (en) * 2018-08-06 2018-11-30 贵州布依仁农业科技有限公司 A kind of oil tea oil expression method
CN109181865A (en) * 2018-11-16 2019-01-11 华中农业大学 A kind of deodorization treatment process of edible oil
CN110951538A (en) * 2019-11-19 2020-04-03 山东华胜检验检测技术有限公司 Physical refining production process of peanut oil
CN112831371A (en) * 2019-11-24 2021-05-25 湖南大三湘茶油股份有限公司 High-quality colorless tea oil and preparation method thereof
CN112831372A (en) * 2019-11-25 2021-05-25 湖南大三湘茶油股份有限公司 Pure camellia oil and preparation method thereof
CN111996076A (en) * 2020-09-10 2020-11-27 江西齐云山油茶科技有限公司 Process for reducing free fatty acid of camellia oil by using enzymatic esterification method
CN112877133A (en) * 2021-01-05 2021-06-01 贵州乔盛生物科技有限公司 Tea oil extraction method

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Application publication date: 20170613