CN107828507A - A kind of camellia seed oil refinement method and equipment - Google Patents
A kind of camellia seed oil refinement method and equipment Download PDFInfo
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- CN107828507A CN107828507A CN201711057468.4A CN201711057468A CN107828507A CN 107828507 A CN107828507 A CN 107828507A CN 201711057468 A CN201711057468 A CN 201711057468A CN 107828507 A CN107828507 A CN 107828507A
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- camellia seed
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- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- 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
- C11B3/12—Refining fats or fatty oils by distillation
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of camellia seed oil refinement method and equipment, it is characterised in that is combined supercritical carbon dioxide extraction equipment and molecular distillation equipment, the advantages of making full use of supercritical carbon dioxide extracting and molecular distillation：Supercritical carbon dioxide extracting temperature is low, separation is selective, and the impurity that oil plant nutritional ingredient keeps and proposed is few；The molecular distillation heat time is short, and separation degree is high, and oil plant heat damage is small and purer after refining, therefore quality can reach pollution-free food level, and indices reach agriculture ministerial standard NY/T 751 2017《Pollution-free food edible vegetable oil》.Whole extractive process is all physical process, does not produce the material of pollution environment, and product is really achieved green without any dissolvent residual.The edible oil of top grade is produced using the present invention, meets the needs of people pursue health, environmental protection, there is very wide prospect.
Description
Technical field
The present invention relates to technical field of agricultural product process, particularly a kind of camellia seed oil refinement method and equipment.
Background technology
Camellia seed oil also known as camellia oil, from plant of theaceae oil tea or Camellia yuansienensis (Oil-tea Camellia)
Mature seed, is one of most ancient traditional woody edible vegetable oil in China, and its aliphatic acid forms, quilt very much like with olive oil
Referred to as " east olive oil ".Generally obtained with the grease refinement method such as milling process, lixiviation process.
Without selectivity, the undesirable constituents that tea seed includes can squeeze milling process oil extracting process in expressing process together with oil
Go out.Lixiviation process has certain selectivity, and the quality index of gained oil is better than expressed oil, but leaching oil has the shortcomings that dissolvent residual.
To improve oil plant quality, there are some solution methods.Chinese patent such as notification number CN102504938B discloses a kind of camellia
Oil cooling squeezing and physical refining process, the technique is using micro-wave vacuum, shelling, cold press, filtering, winterization, molecular distillation, absorption
The steps such as removal of impurities decolouring, produce camellia oil index and are higher than country-level squeezing oil standard.But filtering, absorption cause oil loss big,
Adsorbent is to oil plant secondary pollution, and adsorbent post processing is big for environment pollution, and processing cost is high.And for example notification number
CN104673485 A Chinese patent discloses a kind of technique for removing polycyclic aromatic hydrocarbon pollutant in camellia oil, and the technique uses
Supercritical carbon dioxide extracting, reach the μ g/kg of (α) pyrene of benzo in camellia oil ＜ 2.0, benzo (α) pyrene/benzo (α) anthracene/benzo
(b) the μ g/kg of fluoranthene/＜ 10.0.But requirement index can only be reached using the product of the technology individually.For another example notification number
CN105462680 A Chinese patent discloses camellia oil cold press and molecular distillation equipment and method for producing oil, this method squeezing and
Molecular clock camellia oil, reach state's gauge pressure and squeeze one-level：Oleic acid >=74-87%, acid number≤1.0, peroxide value≤6.0.Pressure
Without selectivity, the undesirable constituents that tea seed includes can squeeze out squeezing method oil extracting process in expressing process together with oil, can reach
Sanitary index it is unsecured.
The content of the invention
In order to overcome the shortcomings of the prior art, the present invention provides a kind of camellia seed oil refinement method.
To achieve the above object, the purpose of the present invention is realized in：A kind of camellia seed oil refinement method, it is characterised in that
Comprise the following steps：
(1) camellia seed kernel is prepared；
(2) primary oil is extracted from camellia seed kernel using supercritical CO 2 extraction technology；Extracting pressure be 20~
40MPa；Extraction temperature is 35~70 DEG C；Extraction time is 1~4h, after extraction, successively through two-stage decompression separation；
(3) molecular distillation technique is used, camellia seed oil is obtained by primary oil is concise by least two-stage molecular distillation.
The two-stage decompression separation of the step (2), separation condition are：One-level decompression separation pressure is 5~12MPa, one-level
Separation temperature is 35~50 DEG C；Second depressurized separating pressure is 4~8MPa, and the second-order separation temperature is 35~50 DEG C.
In described step (3), camellia seed oil is obtained by primary oil is concise by three-level molecular distillation, wherein：One fraction
Sub- distillation pressure is 100~3000Pa, and vapo(u)rizing temperature is 70~130 DEG C, obtains one-level light component and one-level heavy constituent；One-level weight
Component carries out secondary molecules distillation, and secondary molecules distillation pressure is 1~50Pa, and vapo(u)rizing temperature is 120~180 DEG C, obtains two level
Light component and two level heavy constituent；Two level heavy constituent carries out three-level molecular distillation, and three-level molecular distillation pressure is 0.1~10Pa, and three
Level molecule vapo(u)rizing temperature is 130~190 DEG C, obtains three-level light component and three-level heavy constituent, three-level heavy constituent is camellia seed oil.
In the step (1), tea seed low temperature drying is peeled off, obtains camellia seed kernel.
A kind of camellia seed oil refining equipment, it is characterised in that including：
- supercritical carbon dioxide extraction equipment, including the extraction kettle and two-stage separation kettle of pipeline serial communication are passed sequentially through,
Separating still is built with stainless steel cloth filler；
- pass through pipeline and the molecular distillation equipment of supercritical carbon dioxide extraction equipment serial communication, including at least two-stage
Molecular distillation post.
Described stainless steel cloth filler is reticulated and stacked and be molded by STAINLESS STEEL WIRE braiding.
Described separating still includes separation kettle, and separation autoclave body bottom is discharging opening, and middle and upper part is provided with gas outlet, separating still
The outlet of gas outlet and feeding pipe is separated equipped with stainless steel cloth filler in vivo.
At least 1/2 space is equipped with stainless steel cloth filler in described separating still body, and the outlet embedment of feeding pipe is not
Run through in rust steel wire filler or from top to down stainless steel cloth filler.
Described two-stage separation kettle bottom connects with molecular distillation equipment, afterbody separating still middle and upper part and recovery dioxy
Change the connection of carbon storage tank, recovery carbon dioxide storage tank connects with high-pressure pump, heater, extraction kettle successively, forms loop.
Described molecular distillation equipment includes three-level molecular distillation post.
Compared with prior art, the present invention makes full use of the advantages of supercritical carbon dioxide extracting and molecular distillation：It is super to face
Boundary's carbon dioxide abstraction temperature is low, separation is selective, and the impurity that oil plant nutritional ingredient keeps and proposed is few；Molecular distillation
Heat time is short, and separation degree is high, and oil plant heat damage is small and purer after refining, therefore quality can reach pollution-free food level,
Indices reach agriculture ministerial standard NY/T 751-2017《Pollution-free food edible vegetable oil》.Whole extractive process is all physics
Process, does not produce the material of pollution environment, and product is really achieved green without any dissolvent residual.Produced using the present invention
Go out the edible oil of top grade, meet the needs of people pursue health, environmental protection, there is very wide prospect.
Brief description of the drawings
Fig. 1 is the flowage structure schematic diagram of present device；
Fig. 2 is the structural representation of separating still of the present invention；
Fig. 3 is the structural representation of the separating still of another structure type of the present invention.
Embodiment
The present invention is a kind of camellia seed oil refinement method, and it comprises the following steps：
(1) camellia seed kernel is prepared.By tea seed low temperature drying, peel off, obtain camellia seed kernel.
(2) primary oil is extracted from camellia seed kernel using supercritical CO 2 extraction technology；Extracting pressure be 20~
40MPa；Extraction temperature is 35~70 DEG C；Extraction time is 1~4h, and stream of supercritical carbon dioxide amount is 100~2000L/h.Extraction
After taking, successively through two-stage decompression separation.Preferably, described two-stage decompression separation, separation condition are：One-level decompression separation pressure
For 5~12MPa, one-level separation temperature is 35~50 DEG C；Second depressurized separating pressure is 4~8MPa, and the second-order separation temperature is 35
~50 DEG C.
(3) molecular distillation technique is used, camellia seed oil is obtained by primary oil is concise by least two-stage molecular distillation.It is preferred that
, camellia seed oil is obtained by primary oil is concise by three-level molecular distillation, wherein：First order molecular distillation pressure be 100~
3000Pa, vapo(u)rizing temperature are 70~130 DEG C, obtain one-level light component and one-level heavy constituent；One-level heavy constituent carries out secondary molecules
Distillation, secondary molecules distillation pressure are 1~50Pa, and vapo(u)rizing temperature is 120~180 DEG C, obtain two level light component and are recombinated with two level
Point；Two level heavy constituent carries out three-level molecular distillation, and three-level molecular distillation pressure is 0.1~10Pa, and three-level molecular distillation temperature is
130~190 DEG C, three-level light component and three-level heavy constituent are obtained, three-level heavy constituent is camellia seed oil.Light component is divided into restructuring
With first order molecular distill in relative concept, boiling point it is relatively low for light component, boiling point it is higher for heavy constituent.
The principle of the supercritical carbon dioxide extracting used above is the solvability and its density using supercritical fluid
Relation, i.e., influence of the pressure and temperature to supercritical fluid solvability and carry out.Utilize the different solvability pair of fluid
Material to be separated is selectively separated, and the blending constituent of optimal proportion is obtained by control condition (pressure and temperature).
Molecular distillation is that liquid material flows through heating surface with filminess and just completes still-process, and its separation degree is high, energy
Separation is conventional to be not easy separated material；Material heated time is short, typically between several seconds to tens seconds, reduces material thermal decomposition
Chance.
As shown in figure 1, a kind of camellia seed oil refining equipment of the present invention, includes by the overcritical of pipeline serial communication
Carbon dioxide abstraction equipment 1 and molecular distillation equipment 2.
Supercritical carbon dioxide extraction equipment 1, including pass sequentially through extraction kettle 12 and the two-stage separation of pipeline serial communication
Kettle 13,14, separating still 13,14 is built with stainless steel cloth filler 18.
Stainless steel cloth filler 18 be by STAINLESS STEEL WIRE be woven into different shape, density and specification net and it is stacked and
Shaping, it is inert solid material, has the advantages that separative efficiency is high, specific surface area is big, porosity is high, gas-liquid contact is abundant.
Stainless steel cloth filler 18 is applied to the separating still 13,14 of supercritical carbon dioxide extraction equipment, separative efficiency can be improved,
Yield improves.
Separating still 13,14 includes separation kettle 19, and separation kettle 19 bottom is discharging opening 191, and middle and upper part is provided with gas outlet
192, separation kettle 19 separates gas outlet 192 and the outlet 31 of feeding pipe 3 built with stainless steel cloth filler 18, preferably
, the space for separating in kettle 19 at least 1/2 is equipped with stainless steel cloth filler 18.The outlet 31 of feeding pipe 3 is embedded to stainless steel
(as shown in Figure 2) or run through stainless steel cloth filler 18 (as shown in Figure 3) from top to down in wire packing 18.
Carbon dioxide air source 11 connects with high-pressure pump 16, heater 17, extraction kettle 12.Two-stage separation kettle 13,14 bottoms with
Molecular distillation equipment 2 connects, and the middle and upper part of afterbody separating still 14 connects with recovery carbon dioxide storage tank 15, reclaims carbon dioxide
Storage tank 15 connects with high-pressure pump 16, heater 17, extraction kettle 12 successively, forms loop, realizes recycling for carbon dioxide.
Molecular distillation equipment 2 includes at least two-stage molecular distillation post.Preferable molecular distillation equipment 2 as shown in Figure 1
Including three-level molecular distillation post.Two-stage separation kettle 13,14 bottoms connect with the primary oil tank 21 of molecular distillation equipment 2, primary
Oil tank 21 is sequentially communicated with three-level molecular distillation post 22,23,24 again.
Below by way of embodiment, the invention will be further described.
Embodiment 1
As shown in Figure 1 and Figure 2, supercritical carbon dioxide extraction equipment constitutes jointly camellia seed oil with molecular distillation equipment and carried
Equipment is refined, wherein the separating still of supercritical carbon dioxide extraction equipment is built with stainless steel cloth filler.
Tea seed low temperature drying, peels off, and obtains camellia seed kernel；Camellia seed kernel is put into extraction kettle, extracting pressure 28MPa；
Extraction temperature is 55 DEG C；Extraction time is 3h；Stream of supercritical carbon dioxide amount is 1600L/h.One-level decompression separation pressure is
6MPa, one-level separation temperature are 45 DEG C；Second depressurized separating pressure is 4MPa, and the second-order separation temperature is 35 DEG C, obtains primary oil.
Primary oil is heated to 60 DEG C, carries out molecular distillation process, and first order molecular distillation pressure is 200Pa, and first order molecular steams
Temperature is evaporated for 80 DEG C, obtains one-level light component and one-level heavy constituent.
One-level heavy constituent carries out secondary molecules distillation, and secondary molecules distillation pressure is 30Pa, and secondary molecules vapo(u)rizing temperature is
170 DEG C, obtain two level light component and two level heavy constituent.
Two level heavy constituent carries out three-level molecular distillation, and three-level molecular distillation pressure is 0.1Pa, and three-level molecular distillation temperature is
180 DEG C, obtain three-level light component and three-level heavy constituent.Three-level heavy constituent is camellia seed oil.
Embodiment 2
Tea seed low temperature drying, peels off, and obtains camellia seed kernel；Camellia seed kernel is put into extraction kettle, extracting pressure 27MPa；
Extraction temperature is 60 DEG C；Extraction time is 2h；Stream of supercritical carbon dioxide amount is 800L/h.One-level decompression separation pressure is
6MPa, one-level separation temperature are 40 DEG C；Second depressurized separating pressure is 4MPa, and the second-order separation temperature is 35 DEG C, obtains primary oil.
Primary oil is heated to 60 DEG C, carries out molecular distillation process, and first order molecular distillation pressure is 300Pa, and first order molecular steams
Temperature is evaporated for 120 DEG C, obtains one-level light component and one-level heavy constituent.
One-level heavy constituent carries out secondary molecules distillation, and secondary molecules distillation pressure is 10Pa, and secondary molecules vapo(u)rizing temperature is
150 DEG C, obtain two level light component and two level heavy constituent.
Two level heavy constituent carries out three-level molecular distillation, and three-level molecular distillation pressure is 0.1Pa, and three-level molecular distillation temperature is
170 DEG C, obtain three-level light component and three-level heavy constituent.Three-level heavy constituent is camellia seed oil.
Embodiment 3
Tea seed low temperature drying, peels off, and obtains camellia seed kernel；Camellia seed kernel is put into extraction kettle, extracting pressure 25MPa；
Extraction temperature is 65 DEG C；Extraction time is 2h；Stream of supercritical carbon dioxide amount is 400L/h.One-level decompression separation pressure is
5MPa, one-level separation temperature are 35 DEG C；The second-order separation pressure is 4MPa, and second depressurized separation temperature is 35 DEG C, obtains primary oil.
Primary oil is heated to 60 DEG C, carries out molecular distillation process, and first order molecular distillation pressure is 200Pa, and first order molecular steams
Temperature is evaporated for 100 DEG C, obtains one-level light component and one-level heavy constituent.
One-level heavy constituent carries out secondary molecules distillation, and secondary molecules distillation pressure is 5Pa, and secondary molecules vapo(u)rizing temperature is
130 DEG C, obtain two level light component and two level heavy constituent.
Two level heavy constituent carries out three-level molecular distillation, and three-level molecular distillation pressure is 0.1Pa, and three-level molecular distillation temperature is
160 DEG C, obtain three-level light component and three-level heavy constituent.Three-level heavy constituent is camellia seed oil.
Standard GB/T 11765-2003《Camellia seed oil》Sanitary standard press standard GB/T 2716-2005《It is edible to plant
Thing oil sanitary standard》Perform, with agriculture ministerial standard NY/T 751-2017《Pollution-free food edible vegetable oil》Sanitary standard compare
Compared with pollution-free food level requires higher.
The present invention has the characteristics of separation selectivity using supercritical carbon dioxide extracting, by the optimization of technological parameter,
The it is proposed for the undesirable constituents that tea seed includes is effectively prevent, ensures that the impurity of the primary oil of proposition exists from the starting end of flow
Low-level, then being precisely separated by molecular distillation so that quality improves again, and camellia seed oil obtained by embodiment 1-3 reaches
The level of pollution-free food level.
Claims (10)
1. a kind of camellia seed oil refinement method, it is characterised in that comprise the following steps：
(1) camellia seed kernel is prepared；
(2) primary oil is extracted from camellia seed kernel using supercritical CO 2 extraction technology；Extracting pressure is 20~40MPa；
Extraction temperature is 35~70 DEG C；Extraction time is 1~4h, after extraction, successively through two-stage decompression separation；
(3) molecular distillation technique is used, camellia seed oil is obtained by primary oil is concise by least two-stage molecular distillation.
2. camellia seed oil refinement method according to claim 1, it is characterised in that：The two-stage decompression of the step (2) point
From separation condition is：One-level decompression separation pressure is 5~12MPa, and one-level separation temperature is 35~50 DEG C；Second depressurized separates
Pressure is 4~8MPa, and the second-order separation temperature is 35~50 DEG C.
3. camellia seed oil refinement method according to claim 1, it is characterised in that：In described step (3), pass through three-level
Molecular distillation obtains camellia seed oil by primary oil is concise, wherein：First order molecular distillation pressure is 100~3000Pa, vapo(u)rizing temperature
For 70~130 DEG C, one-level light component and one-level heavy constituent are obtained；One-level heavy constituent carries out secondary molecules distillation, and secondary molecules steam
It is 1~50Pa to evaporate pressure, and vapo(u)rizing temperature is 120~180 DEG C, obtains two level light component and two level heavy constituent；Two level heavy constituent is entered
Row three-level molecular distillation, three-level molecular distillation pressure are 0.1~10Pa, and three-level molecular distillation temperature is 130~190 DEG C, is obtained
Three-level light component and three-level heavy constituent, three-level heavy constituent is camellia seed oil.
4. camellia seed oil refinement method according to claim 1, it is characterised in that：It is in the step (1), tea seed is low
Temperature is dried, and is peeled off, is obtained camellia seed kernel.
A kind of 5. camellia seed oil refining equipment, it is characterised in that including：
- supercritical carbon dioxide extraction equipment, including the extraction kettle and two-stage separation kettle of pipeline serial communication are passed sequentially through, separate
Kettle is built with stainless steel cloth filler；
- pass through pipeline and the molecular distillation equipment of supercritical carbon dioxide extraction equipment serial communication, including at least two-stage molecule
Distillation column.
6. camellia seed oil refining equipment according to claim 5, it is characterised in that：Described stainless steel cloth filler is not by
Rust steel wire rod braiding reticulates and stacked and be molded.
7. camellia seed oil refining equipment according to claim 5, it is characterised in that：Described separating still includes separating still
Body, separation autoclave body bottom are discharging opening, and middle and upper part is provided with gas outlet, stainless steel cloth filler is housed by gas outlet in separating still body
Outlet with feeding pipe separates.
8. camellia seed oil refining equipment according to claim 7, it is characterised in that：At least 1/2 in described separating still body
Space stainless steel cloth filler is housed, in the outlet embedment stainless steel cloth filler of feeding pipe or from top to down through stainless
Steel wire filler.
9. camellia seed oil refining equipment according to claim 5, it is characterised in that：Described two-stage separation kettle bottom is with dividing
The connection of sub- distillation equipment, afterbody separating still middle and upper part connect with recovery carbon dioxide storage tank, reclaim carbon dioxide storage tank according to
It is secondary to be connected with high-pressure pump, heater, extraction kettle, form loop.
10. camellia seed oil refining equipment according to claim 5, it is characterised in that：Described molecular distillation equipment includes
Three-level molecular distillation post.
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| CN201711057468.4A CN107828507A (en) | 2017-11-01 | 2017-11-01 | A kind of camellia seed oil refinement method and equipment |
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| CN201711057468.4A CN107828507A (en) | 2017-11-01 | 2017-11-01 | A kind of camellia seed oil refinement method and equipment |
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| CN109456829A (en) * | 2018-11-22 | 2019-03-12 | 西南林业大学 | A kind of preparation method of rubber seed oil |
| CN109868181A (en) * | 2019-03-01 | 2019-06-11 | 临泉县清华地产中药材有限责任公司 | A kind of garlic oil and its process for separation and purification |
| CN111389048A (en) * | 2020-04-30 | 2020-07-10 | 华陆工程科技有限责任公司 | Method for recovering carbon dioxide in supercritical extraction vegetable oil production |
| CN115475400A (en) * | 2022-09-30 | 2022-12-16 | 湘南学院 | Method for removing polycyclic aromatic hydrocarbon in tea oil by molecular distillation |
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| CN109868181A (en) * | 2019-03-01 | 2019-06-11 | 临泉县清华地产中药材有限责任公司 | A kind of garlic oil and its process for separation and purification |
| CN111389048A (en) * | 2020-04-30 | 2020-07-10 | 华陆工程科技有限责任公司 | Method for recovering carbon dioxide in supercritical extraction vegetable oil production |
| CN115475400A (en) * | 2022-09-30 | 2022-12-16 | 湘南学院 | Method for removing polycyclic aromatic hydrocarbon in tea oil by molecular distillation |
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