Treatment method of grease processing trapping liquid, method for increasing nutrient content in grease and grease

Abstract

The invention relates to the field of grease, and discloses a grease processing trapping liquid treatment method, a method for increasing the nutrient content in grease and grease, the treatment method comprises the following steps: carrying out gradient cooling on a grease deodorization trapping liquid at 55-65 DEG C to gradually reduce the temperature to-5-5 DEG C, and keeping the temperature stage for 27-33 hours, according to the method, the grease deodorization trapping liquid is subjected to gradient cooling and is kept at a relatively low temperature for enough time, so that a high-melting-point substance becomes viscous, and impurities in the grease deodorization trapping liquid can be wrapped by the high-melting-point substance in the process, so that the grease deodorization trapping liquid can be fully filtered, and the grease deodorization trapping liquid is prevented from being polluted by the impurities in the grease deodorization trapping liquid. According to the present invention, the oil content is reduced, such that the impurities are reduced, the viscosity of the oil is reduced by heating, the melting point substance and the wrapped impurities in the oil can be conveniently filtered, and the treated substance obtained after filtration contains rich VE and sterol, and can be used for refining crude oil and / or degummed oil so as to achieve the purpose of oil nutrient retention rate increasing.

Description

Technical Field

[0001] The invention relates to the field of oils and fats, and in particular to a method for treating oil processing captured liquid, a method for improving the nutrient content in oils and fats, and the oils and fats. Background Art

[0002] Oil is one of the three major nutrients required by the human body. It can not only provide energy and essential fatty acids for the human body, but also is an important source of fat-soluble vitamins, phytosterols and other functional ingredients for the human body. Vitamin E is a natural antioxidant that can neutralize free radicals, reduce oxidative damage to cells and tissues, and has multiple functions such as improving human immunity, anti-inflammatory, anti-aging, and blood vessel health; phytosterols have the effect of lowering total cholesterol and low-density lipoprotein cholesterol in the human body, helping to reduce the risk of cardiovascular disease. It has been reported that phytosterols have a certain inhibitory effect on the occurrence and development of breast cancer, gastric cancer, intestinal cancer and other cancers.

[0003] The existing method of increasing the nutrient content in oils and fats is mainly to adjust the process parameters of oil production and refining. Guo Shaohai conducted an orthogonal experiment based on the single-factor experiment of steam dosage, oil inlet flow rate and oil inlet temperature and obtained the process conditions with the lowest VE loss in the deodorization process control (Effect of deodorization process control on VE content in oils and fats [J] "China Oils and Fats" 2007, 32 (6): 65-66); Agnieszka et al.'s research showed that the content of fat-soluble vitamin E and phytosterols in the oil extracted from dehulled rapeseed was higher than that of undehulled rapeseed (Dehulling and microwave pretreatment effects on the physicochemical composition and antioxidant capacity of virgin rapeseed oil [J]. Journal of Food Science and Technology, 2017, 54 (3): 627-638). This method of increasing the nutrients in oils and fats is greatly constrained by the quality of raw materials and the advancedness of equipment, and the increase in the content of nutrients such as VE and phytosterols is limited.

[0004] At present, the industry's method for processing deodorized liquid from vegetable oil processing is to first convert the fatty acids that account for the largest proportion of the deodorized liquid into fatty acid methyl esters by the methyl esterification method, and then use the physical property differences between fatty acid methyl esters and VE and sterols such as molecular weight, melting point, and solubility to prepare high-purity VE and sterol products by molecular sorting or solvent extraction. There are few reports on adding VE and sterols in the deodorized liquid back into oils and fats.

[0005] CN 116333816 A reports that the vegetable oil deodorization capture liquid is first subjected to two-stage capture treatment, and then the high-concentration (VE, sterol) deodorization capture liquid is added back to the deodorization or decolorization section to achieve the purpose of increasing the nutrient content. However, the study found that when the oil is treated under high temperature and low pressure conditions in the deodorization section, a series of reactions such as oil hydrolysis, fatty acid oxidation, polymerization, etc. will occur in the oil system, and eventually a small amount of high-melting point unknown substances will exist in the deodorization capture liquid, which may cause the first-level oil after processing to become hazy and have poor quality stability. Summary of the invention

[0006] The purpose of the present invention is to overcome the problem in the prior art that the oil deodorization capture liquid still contains high-melting-point substances after further treatment, and the quality stability of the finished oil is poor after the oil deodorization capture liquid containing the high-melting-point substances is added back to the oil to be processed. A method for treating an oil processing capture liquid and a method and oil for improving the nutrient content in the oil are provided. The oil deodorization capture liquid treated by the method does not contain high-melting-point substances, and after adding it back to the oil to be processed, the prepared finished oil has good stability.

[0007] In order to achieve the above-mentioned purpose, the present invention provides a method for treating oil processing captured liquid, wherein the treatment method comprises: gradually cooling the oil deodorization captured liquid at a temperature of 55-65°C to gradually reduce its temperature to -5°C to 5°C, and maintaining it at this temperature stage for 27-33h, then heating it to 15-25°C, and then filtering it to obtain a treated product of the oil deodorization captured liquid.

[0008] The above technical scheme makes the high-melting-point substance viscous by gradually cooling the oil deodorization collection liquid (also known as oil deodorization distillate in the industry) and keeping it at a relatively low temperature for a sufficient time. In this process, the high-melting-point substance will also wrap the impurities in the oil deodorization collection liquid inside, so that the impurities are also reduced. The temperature is then raised to reduce the viscosity of the oil, making it easy to filter out the high-melting-point substance and the impurities wrapped therein. The treated product obtained after filtration contains rich VE and sterols, and basically does not contain harmful impurities, high-melting-point substances, etc., and reaches the standard of being directly added to crude oil and / or degummed oil.

[0009] The second aspect of the present invention provides a method for improving the nutrient content in oils and fats, wherein the preparation method comprises: adding the processed product of the oil deodorization collection liquid obtained by the processing method described in the first aspect of the present invention to crude oil and / or degummed oil, and the added amount of the processed product of the oil deodorization collection liquid is 0.5-2wt% based on the total amount of the crude oil or degummed oil.

[0010] The third aspect of the present invention provides a fat prepared according to the method of the second aspect of the present invention, wherein, based on the total amount of the fat, the sterol concentration in the fat is 2000-15000 ppm, and / or the vitamin E concentration is 200-1500 ppm.

[0011] Through the above technical scheme, the high-melting-point substances are fully precipitated by gradually cooling the oil deodorization collection liquid and keeping it at a relatively low temperature for a sufficient time. In this process, the high-melting-point substances also wrap the impurities in the oil deodorization collection liquid inside, thereby reducing the impurities. The treated product obtained after filtration contains rich VE and sterols, and basically does not contain harmful impurities, high-melting-point substances, etc., and reaches the standard of being directly added to crude oil and / or degummed oil.

[0012] When the treated material is added back into the crude oil and / or degummed oil, the content of VE and / or sterol in the final finished oil can be significantly increased, thereby increasing the nutrient content of the final finished oil. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 It is a structural schematic diagram of the processing system provided by the present invention.

[0014] Description of Reference Numerals

[0015] 1-tank body; 2-jacket; 3-delivery pump; 4-filter; 5-processed material storage tank; 6-quantity pump; 7-agitator; 8-motor; 9-temperature control space; 10-heat exchange medium storage tank. DETAILED DESCRIPTION

[0016] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0017] In the description of the present invention, it should be understood that the terms "first", "second", etc. are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, a feature defined as "first", "second", etc. may explicitly or implicitly include at least one of the features.

[0018] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral one; it can be a mechanical connection, an electrical connection, or communication with each other; it can be a direct connection, or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements, unless otherwise clearly defined. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0019] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "some examples" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, without contradiction.

[0020] On one hand, the present invention provides a method for treating oil processing captured liquid, wherein the treatment method comprises: gradually cooling the oil deodorization captured liquid at a temperature of 55-65°C to gradually reduce its temperature to -5°C to 5°C, and maintaining this temperature stage for 27-33h, then heating it to raise its temperature to 15-25°C, and then filtering to obtain a treated product of the oil deodorization captured liquid.

[0021] The oil deodorization collection liquid is also called the oil deodorization distillate, which mainly includes fatty acids, vitamin E, sterols and high melting point substances, and also includes components such as aldehydes, ketones, esters, hydrocarbons, etc., wherein, based on the total amount of the oil deodorization collection liquid, the content of fatty acids is 50-80wt%, the content of high melting point substances is 1-10wt%, and the high melting point substances refer to substances with a melting point of not less than 60°C.

[0022] The source of the oil deodorization capture liquid is not particularly limited, and is generally produced in the process of processing vegetable oil. Generally speaking, crude oil is obtained by processing oil, and the crude oil is degummed, neutralized, decolorized or not, and further deodorized to obtain oil deodorization capture liquid (also referred to as oil deodorization distillate in the industry). The temperature of the deodorization stage is generally 200-300°C and the pressure is 0-500Pa to obtain a gaseous deodorization capture liquid. The gaseous deodorization capture liquid is generally further sent to a capture tower and captured by the capture tower to obtain a liquid oil deodorization capture liquid with a temperature of about 60°C (the gaseous deodorization capture liquid can also be cooled by multi-stage heat exchange to obtain a liquid oil deodorization capture liquid). The pressure in the capture tower is the same as that in the deodorization stage. A low-temperature liquid is sprayed in the capture tower, so that the gaseous deodorization capture liquid is dissolved in the low-temperature liquid, and then a liquid grease deodorization capture liquid is obtained. The temperature of the sprayed low-temperature liquid is generally around 30-50°C. The sprayed low-temperature liquid can be the liquid grease deodorization capture liquid captured by the deodorization tower itself (i.e., the grease deodorization capture liquid is self-circulated). When the liquid level in the capture tower reaches a certain height, part of the liquid is drawn out and sent to the next process. The liquid grease deodorization capture liquid can also be further cooled before entering the capture tower to improve the gas-liquid mass transfer efficiency.

[0023] In some embodiments, preferably, the gradient cooling includes a first cooling, a second cooling, a third cooling and a fourth cooling performed in sequence, each of which includes a cooling stage and a holding stage, wherein the holding stage time of the first cooling, the second cooling and the third cooling is independently 0.5-1.5h, and the holding stage time of the fourth cooling is 27-33h.

[0024] In some embodiments, the filtration pressure does not exceed 3 Bar, preferably 1-2 Bar. 1 Bar = 0.1 MPa.

[0025] By gradually lowering the temperature in batches and maintaining the corresponding stage for a sufficient time, the high melting point material becomes viscous (crystallized) due to cooling and can effectively wrap certain impurities inside. The pressure during filtration should not be too high to prevent the oil from overflowing due to squeezing. The holding time in each stage can be any value within the numerical range composed of any two numbers among 0.5h, 0.8h, 1h, 1.2h, and 1.5h.

[0026] In some embodiments, preferably, the difference between the final temperatures of two adjacent cooling steps is 5-20°C.

[0027] In some embodiments, preferably, the temperature of the oil deodorization collection liquid after the first cooling stage is 25-35°C.

[0028] In some embodiments, preferably, the temperature of the oil deodorization collection liquid after the second cooling stage is 15-25°C.

[0029] In some embodiments, preferably, the temperature of the oil deodorization collection liquid after the third cooling stage is 5-15°C.

[0030] In some embodiments, preferably, the temperature of the oil deodorization collection liquid after the fourth cooling stage is -5°C to 5°C.

[0031] During gradient cooling, the temperature after the first cooling can be any value within the numerical range composed of any two numbers among 25°C, 28°C, 30°C, 32°C, and 35°C; the temperature after the second cooling can be any value within the numerical range composed of any two numbers among 15°C, 18°C, 20°C, 22°C, and 25°C; the temperature after the third cooling can be any value within the numerical range composed of any two numbers among 5°C, 8°C, 10°C, 13°C, and 15°C; the temperature after the fourth cooling can be any value within the numerical range composed of any two numbers among -5°C, -2°C, 0°C, 3°C, and 5°C; the temperature after heating can be any value within the numerical range composed of any two numbers among 15°C, 18°C, 20°C, 22°C, and 25°C.

[0032] In some embodiments, preferably, the time required for the cooling stage of the first cooling is 0.5-1 h.

[0033] In some embodiments, preferably, the time required for the cooling stages of the second cooling, the third cooling, and the fourth cooling is independently 0.5-1.5 h.

[0034] In some embodiments, preferably, the time required for heating to the target temperature is 11-13 hours.

[0035] Cooling at the preferred rate is conducive to forming larger crystals of high melting point materials, which can better encapsulate impurities. The time required for the first cooling can be any value within the numerical range of any two of 0.5h, 0.8h, and 1h; the time required for the second to fourth cooling can be any value within the numerical range of any two of 0.5h, 0.8h, 1h, 1.2h, and 1.5h respectively; the time required for heating can be any value within the numerical range of any two of 11h, 12h, and 13h.

[0036] In some embodiments, preferably, the stirring speed of the first cooling is 30-90 rpm.

[0037] In some embodiments, preferably, the stirring speed of the second cooling is 10-70 rpm.

[0038] In some embodiments, preferably, the stirring speed of the third cooling is 10-50 rpm.

[0039] In some embodiments, preferably, the stirring speed of the heating is 10-50 rpm.

[0040] Stirring is required during the cooling and holding stages of each cooling process. Stirring can allow the crystals of high-melting-point substances to come into more complete contact with materials at various locations, which is more conducive to encapsulating impurities.

[0041] In some embodiments, preferably, the oil deodorization collection liquid is a deodorization collection liquid of plant oil, and the plant oil is preferably at least one of corn oil, sunflower oil, soybean oil, peanut oil, rapeseed oil, tea seed oil, sesame oil, linseed oil, olive oil, palm oil, rice oil, linseed oil, cottonseed oil and safflower oil. The method for obtaining the oil deodorization collection liquid may include: obtaining crude oil by squeezing plant seeds, deodorizing the crude oil under the conditions of a deodorization temperature of 200-300°C and a pressure of 0-500Pa, and the liquid captured / collected during the deodorization process is the oil deodorization collection liquid.

[0042] In some embodiments, preferably, the treatment method is carried out in a treatment system, which includes a crystallization tank, a delivery pump and a filter connected in sequence, wherein the gradient cooling and heating are both carried out in the crystallization tank, and the filtration is carried out in the filter.

[0043] In some embodiments, preferably, the crystallization tank comprises a tank body, a stirrer is arranged in the tank body, a jacket is arranged outside the tank body, a temperature control space is formed between the jacket and the tank body, the lower part of the temperature control space is connected to a heat exchange medium storage tank through a heat exchange medium feed pipe, and the upper part of the temperature control space is connected to the heat exchange medium storage tank through a heat exchange medium discharge pipe. When the heat exchange medium flows through the space between the tank body and the jacket, heat exchange can be performed, thereby heating or cooling the material in the tank body. The heat exchange medium is not particularly limited, and can be a mixture of ethylene glycol and / or water, for example.

[0044] In some embodiments, preferably, the delivery pump is connected to the discharge port of the crystallizer through a first delivery pipe, and is connected to the feed port of the filter through a second delivery pipe, and the first delivery pipe and the second delivery pipe are respectively coated with a thermal insulation layer. The thermal insulation layer can be used to insulate the material in the pipeline so that the material state can be maintained for filtration.

[0045] The second aspect of the present invention provides a method for improving the nutrient content in oils and fats, wherein the preparation method comprises: obtaining a processed product of oil deodorization collection liquid according to the processing method described in the first aspect of the present invention, adding the processed product of oil deodorization collection liquid to crude oil and / or degummed oil, and the added amount of the processed product of oil deodorization collection liquid is 0.5-2wt% based on the total amount of crude oil or degummed oil.

[0046] By adopting the above technical scheme, adding an appropriate amount of processed material of oil deodorization collection liquid can effectively increase the nutrient content of finished oil, and the added amount can be any value within the numerical range composed of any two numbers among 0.5wt%, 1wt%, 1.5wt%, and 2wt%.

[0047] After the crude oil and / or degummed oil treated with the added oil deodorization collection liquid is further refined, the finished oil can be obtained, wherein the refining includes one or more procedures of neutralization, decolorization, deodorization, and dewaxing, which can be selected according to the production process requirements. During the neutralization process, the concentration of the sodium hydroxide solution is controlled not to exceed 10-15wt%, and the amount of super alkali is not more than 20wt%; for decolorization, the specific surface area or comprehensive specific surface area can be selected to exceed 150m 2 / g of decolorant or compound decolorant is used for decolorization, and the amount of the decolorant or compound decolorant used does not exceed 4wt% of the total amount of oil and fat; deodorization can be carried out by freezing vacuum deodorization, and the temperature in the deodorization tower is controlled to be 200-300℃ and the pressure is lower than 3mbar; dewaxing can use diatomaceous earth as a filter aid, the dewaxing temperature is 4-8℃, and the time is 10-20h.

[0048] The concentration of sodium hydroxide in the refining stage in the present invention does not exceed 10-15wt% means that the amount of sodium hydroxide does not exceed 10-15wt% based on the total amount of the sodium hydroxide solution.

[0049] The excess alkali amount not exceeding 20wt% means: in addition to the theoretical alkali amount required for neutralization, the excess alkali amount added to achieve the requirement of sufficient removal of free fatty acids is not more than 20wt% based on the total amount of the theoretical alkali amount required for neutralization.

[0050] The third aspect of the present invention provides a fat prepared according to the method of the second aspect of the present invention, wherein, based on the total amount of the fat, the concentration of sterols in the fat is 2000-15000 ppm, and / or the concentration of vitamin E is 200-1500 ppm.

[0051] The present invention will be described in detail below through examples.

[0052] In the following examples, the content of vitamin E in oils and fats is determined according to the second method of GB 5009.82-2016 "National Food Safety Standard for the Determination of Vitamin A, D and E in Foods", the content of sterols in oils and fats is determined according to GB / T 25223-2010 "Determination of Sterol Composition and Total Sterols in Animal and Plant Oils and Fats by Gas Chromatography", and the acid value is determined according to GB 5009.229-2016 "National Food Safety Standard for the Determination of Acid Value in Foods".

[0053] Vitamin E retention rate % = vitamin E content in the product / vitamin E content in the crude oil × 100%.

[0054] Sterol retention rate % = sterol content in the product / sterol content in the crude oil × 100%.

[0055] The processing system structure used in the following embodiments is as follows: Figure 1 As shown, it includes a crystallization tank, a delivery pump 3 and a filter 4 connected in sequence, wherein the gradient cooling and heating are both carried out in the crystallization tank, and the filtration is carried out in the filter 4.

[0056] The crystallization tank comprises a tank body 1, a feed port is provided at the upper portion of the tank body 1, a stirrer 7 is provided inside the tank body 1, the stirrer 7 is connected to a motor 8, a jacket 2 is provided outside the tank body, a temperature control space 9 is formed between the jacket 2 and the tank body 1, the lower portion of the temperature control space 9 is connected to a heat exchange medium storage tank 10 via a heat exchange medium feed pipe, and the upper portion of the temperature control space 9 is connected to the heat exchange medium storage tank 10 via a heat exchange medium discharge pipe.

[0057] The discharge port at the lower part of the tank body 1 is connected to the feed port of the delivery pump 3 through the first delivery pipe, and the discharge port of the delivery pump 3 is connected to the feed port of the filter 4. The filter 4 is a plate and frame filter. The first delivery pipe and the second delivery pipe are respectively coated with insulation layers. The discharge port of the filter 4 is connected to a treated material storage tank 5, and the treated material storage tank 5 is connected to a metering pump 6. When needed, the treated material of the oil deodorization capture liquid is transported to the crude oil and / or post-degummed oil through the metering pump 6.

[0058] The temperature of the deodorized collected liquid produced in oil processing is generally 55-65°C, and the temperature of the deodorized collected liquid used in the present invention is 60°C.

[0059] In the following examples and comparative examples, the preparation method of the oil deodorization collection liquid used is as follows: corn / sunflower seeds / soybeans are processed separately to obtain corresponding crude oils, and the crude oils are deodorized at a deodorization temperature of 240°C and a pressure of 300Pa to obtain a gaseous deodorized distillate after deodorization, and the gaseous deodorized distillate is sent into a collection tower connected thereto, the pressure in the tower is the same as the deodorization pressure, and a low-temperature liquid is sprayed in the tower, and the temperature of the low-temperature liquid is 42°C, so that the gaseous deodorized distillate is absorbed by the low-temperature liquid to obtain the corresponding oil deodorization collection liquid. Based on the total amount of the oil deodorization collection liquid, the content of high melting point substances in the three collection liquids is approximately 5wt%, 4wt%, and 3wt%, respectively. The test method for the content of high melting point substances is as follows: the grease deodorization collection liquid is cooled to -18°C and left overnight (about 18 hours), then allowed to naturally heat up to 0°C, then heated from 0°C to 20°C at a rate of 0.5°C / min, maintained for 0.5 hours, and then a certain amount of the grease deodorization collection liquid is taken for suction filtration, the filtrate is the high melting point substance, and its content is calculated as follows: high melting point substance wt% = mass of the filtrate / mass of the grease deodorization collection liquid to be filtered × 100%.

[0060] In the following examples and comparative examples, the concentration of sodium hydroxide refers to: the amount of sodium hydroxide based on the total amount of sodium hydroxide solution;

[0061] The excess alkali amount refers to the amount of alkali added to meet the theoretical alkali amount required for neutralization in order to fully remove free fatty acids. Based on the total amount of theoretical alkali required for neutralization, the additional amount of alkali added is the excess alkali amount.

[0062] Example 1

[0063] The deodorized collection liquid produced when processing corn was taken, and the contents of vitamin E and sterol in the deodorized collection liquid before treatment were determined. The results are shown in Table 1.

[0064] First cooling: transfer the deodorized collection liquid at 60°C to the crystallizer, turn on the stirrer at 80 rpm, set the water temperature in the jacket to 30°C, stir continuously for 1 hour until the temperature of the deodorized collection liquid in the crystallizer drops to 30°C, adjust the stirrer speed to 60 rpm, and maintain for 1 hour;

[0065] Second cooling: adjust the stirrer speed to 40rpm, set the water temperature in the jacket to drop to 20℃ within 1h, and keep it for 1h when the temperature of the material in the crystallization tank drops to 20℃;

[0066] The third cooling: adjust the stirrer speed to 20rpm, set the water temperature in the jacket to drop to 10°C within 1h, and when the temperature of the material in the crystallization tank drops to 10°C, maintain it for 1h;

[0067] The fourth cooling: turn off the agitator, set the water temperature in the jacket to cool down to 0°C within 1 hour, and keep it for 30 hours when the temperature of the material in the crystallization tank drops to 0°C;

[0068] Heating: Set the water temperature in the jacket to 20°C within 12 hours, turn on the agitator, set the speed to 20 rpm, and after the temperature reaches the set temperature, use the delivery pump 3 to transfer the viscous deodorizing collection liquid to the plate and frame filter for filtration, control the filtration pressure not to exceed 3 Bar, and obtain the treated product of the grease deodorizing collection liquid.

[0069] The results of measuring the content of vitamin E and sterol, extraction rate, etc. of the treated material are shown in Table 1.

[0070] The obtained treated material is added to corn crude oil at 1.5wt% (oil weight), and then neutralized, decolorized, deodorized, dewaxed, and filtered to obtain a corn oil product, wherein the concentration of the sodium hydroxide solution is controlled to be 15wt% and the amount of super alkali is 20wt% during neutralization, and a specific surface area of ​​180m is added during decolorization. 2 / g of a composite decolorizing agent (activated clay + activated carbon, the weight ratio of the two is 9:1), the addition amount is 2.5wt% (based on the total amount of corn crude oil), a freezing vacuum system is used for deodorization, the temperature of the deodorization tank is controlled at 240°C and the pressure is 2.5mbar, the temperature is 4°C and the time is 10h during dewaxing, and diatomaceous earth is used as a filter aid during filtration (the dosage is 0.5wt%).

[0071] The corn oil product obtained has a vitamin E content of 1156.1 ppm, a sterol content of 10800.2 ppm, a sterol retention rate of 100%, a vitamin E retention rate of 98.1%, an acid value of 0.15 mg / g, and no precipitate is produced during the 18-month storage period, and the oil is clear and transparent.

[0072] Example 2

[0073] The deodorized collection liquid produced when processing sunflower seed oil was taken, and the contents of vitamin E and sterol in the deodorized collection liquid before treatment were determined. The results are shown in Table 1.

[0074] First cooling: transfer the deodorized captured liquid with a temperature of 60°C generated during the processing of sunflower oil to a crystallizer, turn on the agitator at a speed of 80 rpm, set the water temperature in the jacket to 30°C, stir continuously for 1 hour until the temperature of the deodorized captured liquid in the crystallizer drops to 30°C, adjust the agitator speed to 60 rpm, and maintain for 1 hour;

[0075] Second cooling: adjust the stirrer speed to 40rpm, set the water temperature in the jacket to drop to 20℃ within 1.5h, and keep it for 1.5h when the temperature of the material in the crystallization tank drops to 20℃;

[0076] The third cooling: adjust the stirrer speed to 20rpm, set the water temperature in the jacket to drop to 10°C within 1.5h, and keep it for 1.5h when the temperature of the material in the crystallization tank drops to 10°C;

[0077] The fourth cooling: turn off the agitator, set the water temperature in the jacket to cool down to 0°C within 1.5h, and keep it for 33h when the temperature of the material in the crystallization tank drops to 0°C;

[0078] Heating: Set the water temperature in the jacket to 20°C within 13 hours, turn on the agitator, set the speed to 20 rpm, and after the temperature reaches the set temperature, use the delivery pump 3 to transfer the viscous deodorizing collection liquid to the plate and frame filter for filtration, control the filtration pressure not to exceed 3 Bar, and obtain the treated product of the grease deodorizing collection liquid.

[0079] The vitamin E and sterol contents of the treated material were determined. The results are shown in Table 1.

[0080] The obtained treated material is added to the crude sunflower seed oil at 0.8wt% (oil weight), and then neutralized, decolorized, deodorized, dewaxed, and filtered to obtain a corn oil product, wherein the concentration of the alkali solution (sodium hydroxide) is controlled to be 10% during neutralization, the amount of super alkali is 10wt%, and a specific surface area of ​​150m is added during decolorization. 2 / g of a composite decolorizer (activated white clay + attapulgite, the weight ratio of the two is 1:1), the addition amount is 0.5wt% (based on the total amount of sunflower seed crude oil), a freezing vacuum system is used for deodorization, the temperature of the deodorization tank is controlled at 240°C and the pressure is 3mbar, the temperature is 8°C and the time is 20h during dewaxing, and diatomaceous earth is used as a filter aid during filtration (the dosage is 0.3wt%).

[0081] The obtained sunflower seed oil product has a vitamin E content of 789.2 ppm, a sterol content of 2991.3 ppm, a vitamin E retention rate of 100%, a sterol retention rate of 99.3%, an acid value of 0.10 mg / g, and no precipitates are present during the 18-month storage period, and the oil is clear and transparent.

[0082] Example 3

[0083] The deodorized liquid collected during the processing of soybean oil was taken and the contents of vitamin E and sterol in the deodorized liquid before treatment were determined. The results are shown in Table 1.

[0084] First cooling: transfer the deodorized captured liquid with a temperature of 60°C generated during the processing of soybean oil to a crystallizer, turn on the agitator at a speed of 80 rpm, set the water temperature in the jacket to 30°C, and continue stirring for 0.5 h until the temperature of the deodorized captured liquid in the crystallizer drops to 30°C, adjust the agitator speed to 60 rpm, and maintain for 0.5 h;

[0085] Second cooling: adjust the stirrer speed to 40rpm, set the water temperature in the jacket to drop to 20℃ within 0.5h, and maintain it for 0.5h when the temperature of the material in the crystallization tank drops to 20℃;

[0086] The third cooling: adjust the agitator speed to 20rpm, set the water temperature in the jacket to drop to 10°C within 0.5h, and when the temperature of the material in the crystallization tank drops to 10°C, maintain it for 0.5h;

[0087] The fourth cooling: turn off the agitator, set the water temperature in the jacket to drop to 0°C within 0.5h, and keep it for 27h when the temperature of the material in the crystallization tank drops to 0°C;

[0088] Heating: Set the water temperature in the jacket to 20°C within 11 hours, turn on the agitator, set the speed to 20 rpm, and after the temperature reaches the set temperature, use the delivery pump 3 to transfer the viscous deodorizing collection liquid to the plate and frame filter for filtration, control the filtration pressure not to exceed 3 Bar, and obtain the treated product of the grease deodorizing collection liquid.

[0089] The vitamin E and sterol contents of the treated material were determined. The results are shown in Table 1.

[0090] The obtained treated material is added to the degummed soybean oil at 1.0 wt% (oil weight), and then neutralized, decolorized and deodorized in sequence to obtain a soybean oil product, wherein the concentration of the alkali solution (sodium hydroxide) is controlled to be 18% during neutralization, the amount of super alkali is 15 wt%, and a specific surface area of ​​180 m is added during decolorization. 2 / g of decolorizing agent (activated white clay), the addition amount is 1.0wt% (based on the total amount of soybean degummed oil), and a freezing vacuum system is used for deodorization, and the temperature of the deodorization tank is controlled at 240°C and the pressure is 2.5mbar.

[0091] The obtained soybean oil product has a vitamin E content of 1106.3 ppm, a sterol content of 2896.1 ppm, a vitamin E retention rate of 100%, a sterol retention rate of 97.3%, an acid value of 0.12 mg / g, and no precipitate is present during the 18-month storage period, and the oil is clear and transparent.

[0092] Example 4

[0093] The deodorized captured liquid produced during the processing of corn oil was treated according to the method of Example 2 in patent CN 116333816 A to obtain a primary treated product of the deodorized captured liquid. The contents of vitamin E and sterols in the primary treated product were determined. The results are shown in Table 1.

[0094] The temperature of the initially treated product is 60° C., and the product is transferred to a crystallization tank and treated in the manner of Example 1 to obtain a treated product of oil deodorization collection liquid.

[0095] The vitamin E and sterol contents of the treated material were determined. The results are shown in Table 1.

[0096] The obtained treated material is added to corn crude oil at 0.9 wt% (oil weight), and then neutralized, decolorized, deodorized, dewaxed, and filtered to obtain a corn oil product, wherein the concentration of the alkali solution (sodium hydroxide) is controlled to be 15% and the amount of super alkali is 18 wt% during neutralization, and a specific surface area of ​​180 m is added during decolorization. 2 / g of a composite decolorizer (activated clay + activated carbon, the weight ratio of the two is 9:1), the addition amount is 2.5wt% (based on the total amount of corn crude oil), a freezing vacuum system is used for deodorization, the temperature of the deodorization tank is controlled at 240°C and the pressure is 2.5mbar, the temperature is 4°C and the time is 10h during dewaxing, and diatomaceous earth is used as a filter aid during filtration (the dosage is 0.5wt%).

[0097] The corn oil product obtained has a vitamin E content of 1402.1 ppm, a sterol content of 10800.2 ppm, a sterol retention rate of 100%, a vitamin E retention rate of 119.0%, an acid value of 0.14 mg / g, and no precipitate is present during the 18-month storage period, and the oil is clear and transparent.

[0098] Example 5

[0099] The source of the deodorized collection liquid is the same as that in Example 1.

[0100] First cooling: transfer the deodorized captured liquid with a temperature of 60°C generated during the processing of corn oil to a crystallizer, turn on the agitator at a speed of 90 rpm, set the water temperature in the jacket to 35°C, stir continuously for 0.75 h until the temperature of the deodorized captured liquid in the crystallizer drops to 35°C, adjust the agitator speed to 50 rpm, and maintain for 1 h;

[0101] Second cooling: adjust the stirrer speed to 50rpm, set the water temperature in the jacket to drop to 25°C within 1h, and maintain it for 1h when the temperature of the material in the crystallization tank drops to 25°C;

[0102] The third cooling: adjust the stirrer speed to 40rpm, set the water temperature in the jacket to cool down to 15℃ within 1h, and keep it for 1h when the temperature of the material in the crystallization tank drops to 15℃;

[0103] The fourth cooling: turn off the agitator, set the water temperature in the jacket to cool down to 5°C within 1 hour, and keep it for 30 hours when the temperature of the material in the crystallization tank drops to 5°C;

[0104] Heating: Set the water temperature in the jacket to 25°C within 12 hours, turn on the agitator, set the speed to 40 rpm, and after the temperature reaches the set temperature, use the delivery pump 3 to transfer the viscous deodorizing collection liquid to the plate and frame filter for filtration, control the filtration pressure not to exceed 3 Bar, and obtain the treated product of the grease deodorizing collection liquid.

[0105] The vitamin E and sterol contents of the treated material were determined. The results are shown in Table 1.

[0106] Then the treated product was added into crude corn oil at 2 wt % (in oil), and then neutralization, decolorization, deodorization, dewaxing and filtration were carried out in sequence according to the method of Example 1 to obtain the corn oil product.

[0107] The corn oil product obtained has a vitamin E content of 1261.8 ppm, a sterol content of 11305.5 ppm, a sterol retention rate of 104.7%, a vitamin E retention rate of 107.1%, an acid value of 0.15 mg / g, and no precipitate is present during the 18-month storage period, and the oil is clear and transparent.

[0108] Example 6

[0109] The source of the deodorized collection liquid is the same as that in Example 1.

[0110] First cooling: transfer the deodorized captured liquid with a temperature of 60°C generated during the processing of corn oil to a crystallizer, turn on the agitator at a speed of 80 rpm, set the water temperature in the jacket to 25°C, stir continuously for 0.75 h until the temperature of the deodorized captured liquid in the crystallizer drops to 25°C, adjust the agitator speed to 50 rpm, and maintain for 1 h;

[0111] Second cooling: adjust the stirrer speed to 20rpm, set the water temperature in the jacket to drop to 15°C within 1h, and maintain it for 1h when the temperature of the material in the crystallization tank drops to 15°C;

[0112] The third cooling: adjust the stirrer speed to 20rpm, set the water temperature in the jacket to cool down to 5°C within 1h, and keep it for 1h when the temperature of the material in the crystallization tank drops to 5°C;

[0113] The fourth cooling: turn off the agitator, set the water temperature in the jacket to -5°C within 1 hour, and keep it for 30 hours when the temperature of the material in the crystallization tank drops to -5°C;

[0114] Heating: Set the water temperature in the jacket to 15°C within 12 hours, turn on the agitator, set the speed to 20 rpm, and after the temperature reaches the set temperature, use the delivery pump 3 to transfer the viscous deodorizing collection liquid to the plate and frame filter for filtration, control the filtration pressure not to exceed 3 Bar, and obtain the treated product of the grease deodorizing collection liquid.

[0115] The vitamin E and sterol contents of the treated material were determined. The results are shown in Table 1.

[0116] Then, the treated product was added back into the crude corn oil at 0.5 wt% (in oil), and then neutralization, decolorization, deodorization, dewaxing and filtration were carried out in sequence according to the method of Example 1 to obtain the corn oil product.

[0117] The corn oil product obtained has a vitamin E content of 998.3 ppm, a sterol content of 10331.6 ppm, a sterol retention rate of 95.7%, a vitamin E retention rate of 84.7%, an acid value of 0.12 mg / g, and no precipitate is present during the 18-month storage period, and the oil is clear and transparent.

[0118] Example 7

[0119] The method of Example 1 is followed, except that the temperature after the first cooling is 40°C, the temperature after the second cooling is 30°C, and the temperature after the third cooling is 15°C.

[0120] The corn oil product obtained has a vitamin E content of 1066.2 ppm, a sterol content of 10420.0 ppm, a sterol retention rate of 96.5%, a vitamin E retention rate of 90.5%, an acid value of 0.10 mg / g, and no precipitate is produced during the 18-month storage period, and the oil is clear and transparent.

[0121] Example 8

[0122] The process is carried out in the manner of Example 1, except that the time used for the first cooling, the second cooling, the third cooling and the fourth cooling is 0.2 h.

[0123] The corn oil product obtained has a vitamin E content of 1076.7 ppm, a sterol content of 10214.3 ppm, a sterol retention rate of 94.6%, a vitamin E retention rate of 91.4%, an acid value of 0.12 mg / g, and no precipitate is produced during the 18-month storage period, and the oil is clear and transparent.

[0124] Example 9

[0125] The process was carried out in the manner of Example 1, except that the stirring speed for the first cooling was 120 rpm, the stirring speed for the second cooling was 90 rpm, the stirring speed for the third cooling was 80 rpm, and the stirring speed for the heating was 80 rpm.

[0126] The corn oil product obtained has a vitamin E content of 1061.3 ppm, a sterol content of 10400.9 ppm, a sterol retention rate of 96.3%, a vitamin E retention rate of 90.1%, an acid value of 0.13 mg / g, and no precipitate is present during the 18-month storage period, and the oil is clear and transparent.

[0127] Comparative Example 1

[0128] The deodorized collection liquid with a temperature of 60° C. generated during the processing of corn oil was added to the crude corn oil at a rate of 1.5 wt % (based on the total amount of crude corn oil), and then neutralization-decolorization-deodorization-dewaxing-filtration were carried out in sequence according to the method of Example 1.

[0129] The content of vitamin E in the processed corn oil is 1165.1 ppm, the content of sterol is 10893.0 ppm, the sterol retention rate is 100.9%, the vitamin E retention rate is 98.9%, and the acid value is 0.20 mg / g. Within the first month of the storage period, specifically within the 20th to 30th day, precipitates appear and the oil becomes hazy.

[0130] Comparative Example 2

[0131] The deodorized captured liquid with a temperature of 60° C. generated during the processing of corn oil was cooled to 20° C. after 20 hours and then filtered. The filtered deodorized captured liquid was added to the crude corn oil at 1.5 wt % (oil weight), and then neutralized - decolorized - deodorized - dewaxed - filtered in the manner of Example 1.

[0132] The final corn oil had a vitamin E content of 1105.2 ppm, a sterol content of 10681.9 ppm, a sterol retention rate of 98.9%, a vitamin E retention rate of 93.8%, and an acid value of 0.16 mg / g. Within the second month of storage, specifically within the 30th to 45th day in each parallel group, precipitates appeared and the oil became hazy.

[0133] Comparative Example 3

[0134] The deodorized captured liquid with a temperature of 60°C generated during the processing of corn oil is cooled to 20°C for 3 hours and then filtered. The filtered deodorized captured liquid is added to the deodorization section of corn oil processing at 1.5wt% (oil weight). A refrigerated vacuum system is used for deodorization, and the pressure of the deodorization tank is controlled at 2.5mbar. Then, dewaxing is carried out at 4°C for 10 hours, and diatomaceous earth is used as a filter aid (the dosage is 0.5wt%).

[0135] The final corn oil had a vitamin E content of 1289.6 ppm, a sterol content of 11345.3 ppm, a sterol retention rate of 105.0%, a vitamin E retention rate of 109.4%, and an acid value of 1.97 mg / g. Within the first month of storage, specifically within 20-30 days in each parallel group, precipitates appeared and the oil became hazy.

[0136] Comparative Example 4

[0137] The primary treated product of the deodorized captured liquid obtained in Example 4 was cooled from 60°C to 20°C for 15 hours and then filtered. The filtered deodorized captured liquid was added to the deodorization section of corn oil processing at 0.7wt% (oil weight). A refrigerated vacuum system was used for deodorization, and the pressure of the deodorization tank was controlled to be 2.5mbar. The deodorized oil was then dewaxed at 4°C for 10 hours, and diatomaceous earth was used as a filter aid (at a dosage of 0.5wt%).

[0138] In the corn oil obtained after processing, the content of vitamin E was 1405.6 ppm, the content of sterol was 11176.2 ppm, the sterol retention rate was 103.5%, the vitamin E retention rate was 119.3%, and the acid value was 1.43 mg / g. Within the second month of the storage period, specifically, in each parallel group within 30-40 days, precipitates appeared and the oil became hazy.

[0139] Comparative Example 5

[0140] The primary treated product of the deodorized captured liquid obtained in Example 4 was cooled from 60°C to 20°C for 5 hours and then filtered. The filtered deodorized captured liquid was added to crude corn oil at 0.9wt% (oil weight), and then neutralized - decolorized - deodorized - dewaxed - filtered in the manner of Example 4 to obtain a corn oil product.

[0141] The corn oil obtained after processing had a vitamin E content of 1234.1 ppm, a sterol content of 10408.2 ppm, a sterol retention rate of 96.4%, a vitamin E retention rate of 104.7%, and an acid value of 0.12 mg / g. Within the first month of the storage period, specifically within the 20th to 30th days in each parallel group, precipitates appeared and the oil became hazy.

[0142] Comparative Example 6

[0143] The process was carried out in the same manner as in Example 1, except that the temperature of the material in the crystallization tank was kept at 0° C. for 20 h.

[0144] The corn oil obtained after processing had a vitamin E content of 1149.8 ppm, a sterol content of 10684.9 ppm, a sterol retention rate of 98.9%, a vitamin E retention rate of 97.6%, and an acid value of 0.13 mg / g. Within the third month of the storage period, specifically within 75-90 days in each parallel group, precipitates appeared and the oil became hazy.

[0145] Comparative Example 7

[0146] The method of Example 1 is followed, except that the temperature is kept at 10° C. for 30 h after the third cooling to 10° C., and then the temperature is directly raised without the fourth cooling.

[0147] In the corn oil obtained after processing, the content of vitamin E was 1116.8 ppm, the content of sterol was 10698.1 ppm, the retention rate of sterol was 99.1%, the retention rate of vitamin E was 94.8%, and the acid value was 0.12 mg / g. Within the 1st to 2nd month of the storage period, specifically within 25-40 days in each parallel group, precipitates appeared and the oil became hazy.

[0148] Comparative Example 8

[0149] The deodorized collection liquid generated during the processing of corn oil is cooled to 25°C at a rate of 0.02°C / min and maintained for 1 hour, then cooled to 5°C at a rate of 0.05°C / min and maintained for 1 hour, then heated to 10°C at a rate of 0.02°C / min and maintained for 1 hour, then cooled to 5°C at a rate of 0.02°C / min and maintained for 1 hour, then filtered according to the method of Example 1 and added to the crude corn oil.

[0150] In the corn oil obtained after processing, the content of vitamin E is 984.6 ppm, the content of sterol is 10089.7 ppm, the retention rate of sterol is 93.4%, the retention rate of vitamin E is 83.5%, and the acid value is 0.10 mg / g. Within the 2nd to 3rd month of the storage period, specifically, each parallel group may produce precipitates and the oil may become hazy within 50 to 60 days.

[0151] Table 1 Nutrient content in deodorized capture liquid before and after treatment

[0152]

[0153]

[0154] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A method for treating oil processing captured liquid, characterized in that: The treatment method comprises: gradually cooling the oil deodorization collection liquid at a temperature of 55-65°C to gradually reduce the temperature to -5°C to 5°C, and maintaining the temperature stage for 27-33 hours, and then heating it to 15-25°C, and then filtering it.

2. The processing method according to claim 1, wherein: The gradient cooling includes a first cooling, a second cooling, a third cooling and a fourth cooling performed in sequence, each of which includes a cooling stage and a holding stage, wherein the holding stages of the first cooling, the second cooling and the third cooling are each independently 0.5-1.5 hours, and the holding stage of the fourth cooling is 27-33 hours; And / or, the filtration pressure does not exceed 3 Bar.

3. The processing method according to claim 2, wherein: The difference between the final temperatures of two consecutive coolings is 5-20℃; And / or, the temperature of the oil deodorization collection liquid after the first cooling stage is 25-35°C; And / or, the temperature of the oil deodorization collection liquid after the second cooling stage is 15-25°C; And / or, the temperature of the oil deodorization collection liquid after the third cooling stage is 5-15°C; And / or, the temperature of the oil deodorization collection liquid after the fourth cooling stage is -5°C to 5°C.

4. The processing method according to claim 2 or 3, wherein: The time required for the cooling stage of the first cooling is 0.5-1h; And / or, the time required for the cooling phases of the second cooling, the third cooling, and the fourth cooling is independently 0.5-1.5h; And / or, the time required for heating to the target temperature is 11-13 hours.

5. The processing method according to any one of claims 2 to 4, wherein: The stirring speed of the first cooling is 30-90rpm; And / or, the stirring speed of the second cooling is 10-70 rpm; And / or, the stirring speed of the third cooling is 10-50 rpm; And / or, the stirring speed of the heating is 10-50 rpm; And / or, the oil deodorization collection liquid is a deodorization collection liquid of vegetable oil, and the vegetable oil is preferably at least one of corn oil, sunflower oil, soybean oil, peanut oil, rapeseed oil, tea seed oil, sesame oil, linseed oil, olive oil, palm oil, rice oil, linseed oil, cottonseed oil and safflower oil.

6. The processing method according to any one of claims 1 to 5, wherein: The treatment method is carried out in a treatment system, which includes a crystallization tank, a delivery pump and a filter connected in sequence, wherein the gradient cooling and heating are both carried out in the crystallization tank, and the filtration is carried out in the filter.

7. The processing method according to claim 6, wherein: The crystallization tank comprises a tank body, an agitator is arranged in the tank body, a jacket is arranged outside the tank body, a temperature control space is formed between the jacket and the tank body, the lower part of the temperature control space is connected to a heat exchange medium storage tank through a heat exchange medium feed pipe, and the upper part of the temperature control space is connected to the heat exchange medium storage tank through a heat exchange medium discharge pipe.

8. The processing method according to claim 6 or 7, wherein: The delivery pump is connected to the discharge port of the crystallizer through a first delivery pipe, and is connected to the feed port of the filter through a second delivery pipe. The first delivery pipe and the second delivery pipe are respectively coated with a heat preservation layer.

9. A method for increasing the nutrient content in oils and fats, characterized in that: The method comprises: obtaining a processed product of grease deodorization collection liquid according to the processing method described in any one of claims 1 to 8, adding the processed product of grease deodorization collection liquid to crude oil and / or degummed oil, wherein the added amount of the processed product of grease deodorization collection liquid is 0.5-2wt% based on the total amount of crude oil or degummed oil.

10. A grease prepared according to the method of claim 9, characterized in that: Based on the total amount of the oil, the concentration of sterol in the oil is 2000-15000 ppm, and / or the concentration of vitamin E is 200-1500 ppm.

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