CN111349513B - Processing technology for controlling generation of 3-MCPD ester and glycidyl ester in edible oil - Google Patents
Processing technology for controlling generation of 3-MCPD ester and glycidyl ester in edible oil Download PDFInfo
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- CN111349513B CN111349513B CN202010170379.6A CN202010170379A CN111349513B CN 111349513 B CN111349513 B CN 111349513B CN 202010170379 A CN202010170379 A CN 202010170379A CN 111349513 B CN111349513 B CN 111349513B
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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
- 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
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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Abstract
The invention belongs to the technical field of edible oil processing, and relates to a processing technology for controlling generation of 3-MCPD ester and glycidyl ester in edible oil, which comprises the following steps: (1) Filtering the crude oil, adding a mixed auxiliary agent, stirring and mixing at normal temperature, performing ultrasonic treatment, and performing centrifugal separation to obtain an oil phase; (2) Adding a mixed auxiliary agent into the oil phase obtained in the step (1), stirring and mixing at normal temperature, performing ultrasonic treatment, and performing centrifugal separation to obtain an oil phase; repeating the operation for 6 times; (3) Adding silica gel into the oil phase edible oil obtained after centrifugation in the step (2) for degumming, performing centrifugal separation to obtain an oil phase, repeating twice, filtering the obtained oil phase, decoloring, performing secondary filtration, deodorizing the edible oil at low temperature, and then entering a deacidification device for low-temperature rapid deacidification to obtain the finished oil. The process can remove the plasticizer in the early stage, and a high-temperature distillation step is not required in the later stage, so that the formation of glycidyl ester and 3-MCPD ester caused by high temperature is avoided.
Description
Technical Field
The invention belongs to the technical field of edible oil processing, and particularly relates to a processing technology for controlling generation of 3-MCPD ester and glycidyl ester in edible oil.
Background
At present in agricultural production, the use of a large amount of plastic films for during plasticizer passes through soil migration entering oil, the burning of a large amount of plastic products rubbish in addition leads to the air to be contaminated by plasticizer, thereby makes the oil contaminated by the plasticizer in the air at the planting process, causes edible oil plasticizer too high. The plasticizer is a general name of phthalate, is a chemical high polymer material auxiliary agent, is also called as a plasticizer, has strong toxicity to liver, kidney, lung, heart, reproductive system and the like, and has risks of teratogenesis, carcinogenesis, immunosuppression and the like. At present, most of edible crude oil contains plasticizers which are seriously out of standard, wherein the sources of the plasticizers mainly comprise environmental pollution, non-compliant plastic packaging materials, irregular processing processes and the like. The plasticizer is fat-soluble and is mutually soluble with the edible oil, in the prior art, the fat processing technology mostly adopts high-temperature distillation to remove the plasticizer, but the edible oil after high temperature is easy to produce 3-MCPD ester and glycidyl ester. 3-MCPD ester and glycidyl ester enter a human body to form 3-chloropropanediol and glycidol, and both hazards are internationally recognized genetic carcinogens. In common vegetable oil esters, due to the fact that the refining temperature is too high, the content of 3-MCPD esters and glycidyl esters in the edible oil is far beyond the safety standard, and therefore, an optimized edible oil processing technology is urgently needed, the plasticizer is removed, and meanwhile the generation of the 3-MCPD esters and the glycidyl esters is controlled, so that the safety of the edible oil is improved. In the determination of phthalate in food of national standard GB 5009.271, the detection method of 18 phthalate substances is specified.
The existing method for removing the plasticizer mainly comprises a physical adsorption removal method and a high-temperature distillation removal method. Physical adsorption and removal are carried out by adopting an adsorbent, in the patent with the publication number of CN109880688A, physical adsorption of activated carbon, silicate, activated alumina, activated clay and the like only has an effect on a plurality of phthalic acid esters with small content, but has no obvious effect on common harmful dibutyl phthalate (DBP), di (2-ethylhexyl) phthalate (DEHP) and diisononyl phthalate (DINP). And when the 3-MCPD ester and the glycidyl ester (CN 104694250A) are removed by physical adsorption, foreign matters are easily introduced by physical adsorption, so that the risk and the processing cost are increased. In the method for removing the plasticizer by high-temperature distillation, the high temperature adopted is higher than 250 ℃ (CN 105925371A), which can cause the generation of 3-MCPD ester and glycidyl ester.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a processing technology for controlling the generation of 3-MCPD ester and glycidyl ester in edible oil, which can remove plasticizer in the early stage of the processing technology and does not need a high-temperature distillation step in the later stage, thereby avoiding the formation of glycidyl ester and 3-MCPD ester caused by high temperature.
The technical scheme of the invention is as follows:
a process for controlling the production of 3-MCPD esters and glycidyl esters in edible oils comprising the steps of:
(1) Filtering the crude oil, adding a mixed auxiliary agent into the filtered crude oil, stirring and performing ultrasonic treatment at normal temperature, performing centrifugal separation, and removing subnatant to obtain an oil phase;
(2) Adding a mixed auxiliary agent into the oil phase obtained in the step (1), stirring and mixing at normal temperature, performing ultrasonic treatment, and performing centrifugal separation to obtain an oil phase; repeating the operation for 6 times;
(3) Adding silica gel into the oil-phase edible oil obtained after centrifugation in the step (2) for degumming, performing centrifugal separation to obtain an oil phase, repeating twice, filtering the obtained oil phase, decoloring, performing secondary filtration, deodorizing the edible oil at low temperature, and then entering a deacidification device for low-temperature rapid deacidification to obtain the finished oil.
In the steps, the plasticizer is not well adsorbed due to poor intersolubility of water, activated clay and silica gel with the oil, and the plasticizer in the oil is extracted out by alcohol and is mutually dissolved with water, so that the content of the plasticizer in the oil phase is greatly reduced; the plasticizer dissolved in the alcohol is adsorbed and removed under the synergistic action of the silica gel and the activated clay, and the removal rate of the plasticizer is up to more than 90 percent through filtration and repeated action.
Further, the components of the mixing auxiliary agent comprise water, activated clay, silica gel and alcohol; sequentially adding water, activated clay, silica gel and alcohol into the crude oil, wherein the weight of each component is as follows: weighing water in an amount of 15-20% of the weight of the crude oil, weighing activated clay in an amount of 0.5-1.5 per mill of the weight of the crude oil, weighing silica gel in an amount of 0.5-2.0 per mill of the weight of the crude oil, and weighing alcohol in an amount of 2.0-4.0% of the weight of the crude oil.
Further, the stirring time is 25-35 min, and the ultrasonic time is 25-35 min.
Further, the addition amount of the silica gel in the step (3) is one thousandth of the mass of the oil phase.
Further, the deodorization temperature in the step (3) is 230-245 ℃, and the deodorization time is 12-18 min.
Further, the deacidification temperature in the step (3) is 220-240 ℃.
The invention has the beneficial effects that:
because the crude oil contains the plasticizer, the plasticizer is removed at high temperature in the prior art, and the generation of glycidyl ester and 3-MCPD ester can be caused. The edible oil obtained by adopting the process steps of the invention meets the regulation that 3-MCPD in FDA recommended food should not exceed 1mg/kg dry matter.
Drawings
FIG. 1 is a process flow diagram provided by an embodiment of the present invention.
Detailed Description
The technical solutions of the present invention will be described in detail and fully with reference to the following specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the present invention.
For a further understanding of the present invention, reference will now be made in detail to the present invention with reference to the following examples.
Example 1
A process for controlling the production of 3-MCPD esters and glycidyl esters in edible oils, comprising the steps of:
(1) Filtering the crude oil, and adding a mixed auxiliary agent into the crude oil, wherein the mixed auxiliary agent comprises water, activated clay, silica gel and alcohol; sequentially adding 18%, 1.0% and 4.0% of the crude oil into the crude oil, stirring at normal temperature for 25-35 min, performing ultrasonic treatment for 25-35 min, centrifuging, and removing subnatant to obtain an oil phase;
(2) Adding the mixed auxiliary agent obtained in the step (1) into the oil phase obtained in the step (1), stirring for 25-35 min at normal temperature, mixing, performing ultrasonic treatment for 25-35 min, and performing centrifugal separation to obtain an oil phase; repeating the operation for 6 times;
(3) Adding one thousandth of silica gel of the weight of the edible oil into the oil-phase edible oil obtained after centrifugation in the step (2), degumming, performing centrifugal separation to obtain an oil phase, repeating twice, filtering the obtained oil phase, decoloring, filtering again, heating the filtered edible oil to 230 ℃, performing low-temperature deodorization for 12-18 min, then entering a deacidification device, setting the deacidification temperature at 220 ℃, performing low-temperature rapid deacidification, wherein the deacidification time is 25-30 s, and performing deacidification and cooling to obtain a finished oil product, namely the finished oil product with high safety.
Example 2
A process for controlling the production of 3-MCPD esters and glycidyl esters in edible oils, comprising the steps of:
(1) Filtering the crude oil, and adding a mixed auxiliary agent into the crude oil, wherein the mixed auxiliary agent comprises water, activated clay, silica gel and alcohol; adding the components into the crude oil according to the weight of 15%, 0.5% and 2.0% of the crude oil in turn, stirring at normal temperature for 25-35 min, performing ultrasonic treatment for 25-35 min, performing centrifugal separation, and removing subnatant to obtain an oil phase;
(2) Adding the mixed auxiliary agent obtained in the step (1) into the oil phase obtained in the step (1), stirring for 25-35 min at normal temperature, mixing, performing ultrasonic treatment for 25-35 min, and performing centrifugal separation to obtain an oil phase; repeating the operation for 6 times;
(3) Adding one thousandth of silica gel of the weight of the edible oil into the oil-phase edible oil obtained after centrifugation in the step (2), degumming, performing centrifugal separation to obtain an oil phase, repeating twice, filtering the obtained oil phase, decoloring, filtering again, heating the filtered edible oil to 245 ℃, performing low-temperature deodorization for 12-18 min, then entering a deacidification device, setting the deacidification temperature to 240 ℃, performing low-temperature rapid deacidification, and performing deacidification and cooling for 25-30 s to obtain the finished oil, thus obtaining the finished oil with high safety.
Example 3
A process for controlling the production of 3-MCPD esters and glycidyl esters in edible oils, comprising the steps of:
(1) Filtering the crude oil, and adding a mixed auxiliary agent into the crude oil, wherein the mixed auxiliary agent comprises water, activated clay, silica gel and alcohol; sequentially adding the components into the crude oil according to the weight of 20%, 1.5%, 2.0% and 3.0% of the crude oil respectively, stirring at normal temperature for 25-35 min, performing ultrasonic treatment for 25-35 min, then performing centrifugal separation on the mixture, and removing subnatant to obtain an oil phase;
(2) Adding the mixed auxiliary agent obtained in the step (1) into the oil phase obtained in the step (1), stirring for 25-35 min at normal temperature, mixing, performing ultrasonic treatment for 25-35 min, and performing centrifugal separation to obtain an oil phase; repeating the operation for 6 times;
(3) And (3) adding one thousandth of silica gel of the weight of the edible oil into the oil-phase edible oil obtained after centrifugation in the step (2), degumming, performing centrifugal separation to obtain an oil phase, repeating twice, filtering the obtained oil phase, decoloring, filtering again, heating the filtered edible oil to 235 ℃, performing low-temperature deodorization for 12-18 min, then entering a deacidification device, setting the deacidification temperature to be 230 ℃, performing low-temperature rapid deacidification for 25-30 s, and performing deacidification and cooling to obtain a finished oil product, namely the finished oil product with high safety.
The above description is only for the preferred embodiment of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements and the like made within the scope of the present invention should be included in the patent protection scope of the present invention.
Claims (5)
1. The processing technology for controlling the generation of the 3-MCPD ester and the glycidyl ester in the edible oil is characterized by comprising the following steps:
(1) Filtering the crude oil, adding a mixed auxiliary agent, stirring and mixing at normal temperature, performing ultrasonic treatment, and performing centrifugal separation to obtain an oil phase;
the mixed auxiliary agent comprises water, activated clay, silica gel and alcohol; the components are respectively added into the crude oil according to 15 to 20 percent, 0.5 to 1.5 thousandths, 0.5 to 2.0 thousandths and 2.0 to 4.0 percent of the weight of the crude oil in turn;
(2) Adding a mixed auxiliary agent into the oil phase obtained in the step (1), stirring and mixing at normal temperature, performing ultrasonic treatment, and performing centrifugal separation to obtain an oil phase; repeating the operation for 6 times;
(3) Adding silica gel into the oil phase edible oil obtained after centrifugation in the step (2) for degumming, performing centrifugal separation to obtain an oil phase, repeating twice, filtering the obtained oil phase, decoloring, performing secondary filtration, deodorizing the edible oil at low temperature, and then entering a deacidification device for low-temperature rapid deacidification to obtain the finished oil.
2. The process according to claim 1, wherein the stirring time is 25 to 35min and the ultrasound time is 25 to 35min.
3. The process according to claim 1, wherein the amount of silica gel added in step (3) is one thousandth of the mass of the oil phase.
4. The process according to claim 1, wherein the deodorization temperature in the step (3) is 230 to 245 ℃ and the deodorization time is 12 to 18min.
5. The process according to claim 1, wherein the deacidification temperature in step (3) is 220 to 240 ℃.
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| CN111349513B true CN111349513B (en) | 2023-03-17 |
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| JP5700503B2 (en) * | 2009-09-07 | 2015-04-15 | 日清オイリオグループ株式会社 | Glyceride composition and method for producing the glyceride composition |
| CN102334563B (en) * | 2010-07-16 | 2015-03-25 | 丰益(上海)生物技术研发中心有限公司 | Method for controlling content of 3-chloro-1,2-propanediol or ester thereof in oil |
| CN102533441B (en) * | 2012-01-21 | 2014-01-15 | 上海好油工业设备有限公司 | Degumming process for edible vegetable oil and application thereof |
| CN103908946B (en) * | 2013-01-07 | 2018-04-06 | 丰益(上海)生物技术研发中心有限公司 | A kind of mixed adsorbent, grease and preparation method thereof |
| CN103382413B (en) * | 2013-07-16 | 2015-03-11 | 傅武胜 | Refining process for reducing content of MCPD in tea seed oil |
| CN104694250B (en) * | 2013-12-10 | 2020-02-04 | 丰益(上海)生物技术研发中心有限公司 | Method for reducing 3-MCPD ester and/or glycidyl ester in grease |
| CN105176676A (en) * | 2015-07-17 | 2015-12-23 | 广州市正德生物科技有限公司 | Edible plant oil non-soap refining method |
| CN108239573A (en) * | 2016-12-27 | 2018-07-03 | 中粮集团有限公司 | Grease and preparation method thereof |
| CN107090353B (en) * | 2017-05-04 | 2021-03-09 | 辽宁晟麦实业股份有限公司 | Method for reducing content of glycidyl ester in refined vegetable oil |
| CN110760377A (en) * | 2019-11-15 | 2020-02-07 | 湖南省康多利油脂有限公司 | Preparation method of plasticizer-removed tea oil |
| CN110760382A (en) * | 2019-12-10 | 2020-02-07 | 海南省粮油科学研究所 | Refining method of crabapple seed crude oil |
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