CN113122384A - Method for improving frost resistance of grease - Google Patents

Method for improving frost resistance of grease Download PDF

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Publication number
CN113122384A
CN113122384A CN201911414851.XA CN201911414851A CN113122384A CN 113122384 A CN113122384 A CN 113122384A CN 201911414851 A CN201911414851 A CN 201911414851A CN 113122384 A CN113122384 A CN 113122384A
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particle size
oil
microns
size range
size distribution
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CN113122384B (en
Inventor
朱振南
王勇
刘吕睿
王鑫
周耀琦
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Wilmar Shanghai Biotechnology Research and Development Center Co Ltd
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Wilmar Shanghai Biotechnology Research and Development Center Co Ltd
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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
    • 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
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases
    • 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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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention provides a method for improving the frost resistance of grease. Specifically, the decolorizer with the particle size distribution range of 0.1-100 microns, the median particle size range of 1-30 microns and the deviation value of particle size distribution of-0.3-1 is used for decolorizing the grease to be decolorized, so that the freezing time of the grease can be prolonged, and the frost resistance of the grease can be improved.

Description

Method for improving frost resistance of grease
Technical Field
The invention relates to a method for improving the frost resistance of grease.
Background
The freezing resistance of fats and oils is the ability of the fats and oils to remain clear at low temperatures and is often evaluated by the freezing test of the fats and oils. Wax lipid and lipid contained in the crude rice bran oil are not easy to remove in the refining process, so that the finished oil gradually has solid precipitation in the placing process, becomes turbid and finally precipitates at the bottom, and the appearance of the product is greatly influenced. As the amount of precipitates increases, a colloidal state gradually develops, the fluidity of the oil and fat deteriorates, the digestibility decreases, and the palatability and the odor are affected.
The rice oil is extracted from rice bran and rice germ which are byproducts of rice processing, and the fatty acid composition of the rice oil is close to the composition ratio of good oil recommended by the World Health Organization (WHO). In addition, it inherits many nutrient elements contained in rice, such as oryzanol, phytosterol, vitamin E, etc. Due to the particularity of the oil, the extraction and preparation of the rice bran oil are always very complicated and complicated work, and impurities which are not edible or influence the quality are often difficult to remove, so that the subsequent refining step is difficult and serious, and the quality of the final product is greatly reduced. For example, CN106167738A discloses a method for refining high phytosterol rice oil, which comprises deacidifying crude oil, performing four-stage molecular distillation, dewaxing, deodorizing, and performing flash evaporation and dehydration to obtain the final rice oil. The freezing time of the obtained rice oil can reach more than 24 hours.
CN107746746A discloses a method and a device for improving the quality of vegetable oil, which can further improve the dewaxing and winterization effects of the wax-containing vegetable oil in the crystallization and crystal growing process, and increase the freezing time of the vegetable oil to more than 60 hours, and can be applied to rice oil. According to the invention, oil dewaxing is carried out by adopting eight-stage gradual cooling crystallization, six-stage constant temperature crystal growing and two-stage low temperature filtration methods, and special crystallization and crystal growing equipment is adopted, so that the interference of equipment transmission on the crystallization and crystal growing processes is effectively solved in a comprehensive and synergetic manner.
CN108795573A discloses a method for degreasing and cooling rice bran oil, which comprises the steps of controlling the cooling rate when the temperature of the oil is reduced to 20-3 ℃, then continuously growing crystals for 12 hours at 3 ℃, and degreasing at 5-8 ℃. Controlling the filtering pressure to be 0.1MPA, filtering the oil for the first time, then recrystallizing and filtering to obtain the finished product of rice bran oil. This method facilitates crystallization of the lipid and detection by freeze test.
Disclosure of Invention
The invention aims to improve the freezing time of the grease and the frost resistance of the grease. The invention uses specific decolorant to carry out reaction decoloration in the decoloration process, thereby realizing the effect.
Specifically, the invention provides a method for decoloring oil, which comprises the step of decoloring the oil to be decolored by using a decoloring agent with a particle size distribution range of 0.1-100 microns, a median particle size range of 1-30 microns and a deviation value of particle size distribution of-0.3-1.
In one or more embodiments, the decolorizing agent is selected from the group consisting of activated clay, attapulgite, zeolite, acidified rice hull ash, magnesium silicate, diatomaceous earth, perlite, activated carbon, and any mixtures thereof.
In one or more embodiments, the decolorizing agent is a mixture of activated clay and other decolorizing agents.
In one or more embodiments, the decolorizing agent comprises a mixture of activated clay and one or more decolorizing agents selected from the group consisting of diatomaceous earth, magnesium silicate, activated carbon, and perlite.
In one or more embodiments, the decolorizing agent has a median particle size in the range of 3 to 30 μm.
In one or more embodiments, the decolorizing agent has a median particle size in the range of 5 to 15 μm.
In one or more embodiments, the particle size distribution of the color destroying agent has a deviation value in the range of-0.3 to-0.9.
In one or more embodiments, the particle size distribution of the decolorizing agent has a deviation value of from-0.5 to-0.9, more preferably from-0.7 to-0.9.
In one or more embodiments, the decolorizing agent is used in an amount of 1 to 5%, preferably 2 to 4%, by weight of the oil.
In one or more embodiments, the grease is one that requires improved freeze resistance.
In one or more embodiments, the oil is rice oil, cottonseed oil, soybean oil, sunflower oil, corn oil, or any mixture thereof.
In one or more embodiments, the fat to be decolorized has not been subjected to dewaxing treatment.
In one or more embodiments, the decolorization is performed at a temperature of 100 ℃ and 120 ℃.
In one or more embodiments, the decolorization time is from 10 to 60 minutes.
The invention also provides a method for refining the oil, which comprises the step of decoloring by using the decoloring method before the dewaxing and/or degreasing steps.
In one or more embodiments, the fat refining process comprises decolorizing prior to degreasing using the decolorizing process described herein.
In one or more embodiments, the oil refining process further comprises one or more steps of degumming, deacidification, neutralization, and deodorization.
The invention also provides application of the grease decoloring method in improving grease freezing time.
In one or more embodiments, the grease is one that requires improved freeze resistance.
In one or more embodiments, the oil is rice oil, cottonseed oil, soybean oil, sunflower oil, corn oil, or any mixture thereof.
In one or more embodiments, the fat to be decolorized has not been subjected to dewaxing treatment.
The invention also provides the application of the decolorizing agent with the particle size distribution range of 0.1-100 microns, the median particle size range of 1-30 microns and the deviation value of the particle size distribution of-0.3-1 in improving the oil freezing time.
In one or more embodiments, the application is in decolorization.
In one or more embodiments, the decolorizing agent is selected from the group consisting of activated clay, attapulgite, zeolite, acidified rice hull ash, magnesium silicate, diatomaceous earth, perlite, activated carbon, and any mixtures thereof.
In one or more embodiments, the decolorizing agent is a mixture of activated clay and other decolorizing agents.
In one or more embodiments, the decolorizing agent comprises a mixture of activated clay and one or more decolorizing agents selected from the group consisting of diatomaceous earth, magnesium silicate, activated carbon, and perlite.
In one or more embodiments, the decolorizing agent has a median particle size in the range of 3 to 30 μm.
In one or more embodiments, the decolorizing agent has a median particle size in the range of 5 to 15 μm.
In one or more embodiments, the particle size distribution of the color destroying agent has a deviation value in the range of-0.3 to-0.9.
In one or more embodiments, the particle size distribution of the decolorizing agent has a deviation value of from-0.5 to-0.9, more preferably from-0.7 to-0.9.
Also provided is a decolorizing agent which is characterized in that the particle size distribution range is 0.1-100 microns, the median particle size range is 1-30 microns, and the deviation value of the particle size distribution is-0.3-1.
In one or more embodiments, the decolorizing agent is selected from the group consisting of activated clay, attapulgite, zeolite, acidified rice hull ash, magnesium silicate, diatomaceous earth, perlite, activated carbon, and any mixtures thereof.
In one or more embodiments, the decolorizing agent is a mixture of activated clay and other decolorizing agents.
In one or more embodiments, the decolorizing agent comprises a mixture of activated clay and one or more decolorizing agents selected from the group consisting of diatomaceous earth, magnesium silicate, activated carbon, and perlite.
In one or more embodiments, the decolorizing agent has a median particle size in the range of 3 to 30 μm.
In one or more embodiments, the decolorizing agent has a median particle size in the range of 5 to 15 μm.
In one or more embodiments, the particle size distribution of the color destroying agent has a deviation value in the range of-0.3 to-0.9.
In one or more embodiments, the particle size distribution of the decolorizing agent has a deviation value of from-0.5 to-0.9, more preferably from-0.7 to-0.9.
Detailed Description
To make the features and effects of the present invention comprehensible to those skilled in the art, general description and definitions are made below with reference to terms and expressions mentioned in the specification and claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The theory or mechanism described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features defined herein as numerical ranges or percentage ranges, such as values, amounts, levels and concentrations, are for brevity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to cover and specifically disclose all possible subranges and individual numerical values (including integers and fractions) within the range. Herein, unless otherwise specified, percentages refer to mass percentages and ratios to mass ratios.
In this context, for the sake of brevity, not all possible combinations of features in the various embodiments or examples are described. Therefore, the respective features in the respective embodiments or examples may be arbitrarily combined as long as there is no contradiction between the combinations of the features, and all the possible combinations should be considered as the scope of the present specification.
In this context, the starting materials mentioned may, unless otherwise indicated, be those conventional in the art, and the processes mentioned may be those conventionally carried out in the art, as reasonably determined by the skilled person from the disclosure and the prior art.
The invention discovers that the specific decolorizing agent is used for reaction and decolorization in the decolorizing process, so that the freezing time of the grease can be delayed, and the frost resistance of the grease can be improved. The specific decolorant of the invention has the following characteristics: the particle size distribution range is 0.1-100 microns, the median particle size range is 1-30 microns, and the deviation value of the particle size distribution is-0.3-1. The preferable median particle diameter range is 3 to 30 μm. In some embodiments, the decolorizing agents used in the present invention have a median particle size in the range of 5 to 15 μm. In the present invention, the deviation value of the particle size distribution is preferably-0.3 to-0.9. In some embodiments, the particle size distribution of the decolorizing agents used in the present invention has a deviation value of-0.5 to-0.9, preferably-0.7 to-0.9. In the present invention, the particle size distribution range, the median particle size range, and the deviation value are measured and calculated as described in the examples section.
The present invention can be practiced using various decolorants known in the art for use in the decolorization of fats and oils. Exemplary decolorizing agents include, but are not limited to, activated clay, attapulgite, zeolite, acidified rice hull ash, magnesium silicate, diatomaceous earth, perlite, and activated carbon. One decolorizing agent or any mixture of two or more decolorizing agents can be used. When two or more decolorizing agents are used, there is no particular limitation on the amount ratio between the individual decolorizing agents in the decolorizing agent mixture, as long as the particle size distribution range, median particle size range, and deviation value of the final decolorizing agent are within the ranges defined herein. Exemplary decolorizing agents can be mixtures of activated clay and perlite, perlite and activated carbon, magnesium silicate and diatomaceous earth, and activated clay and other decolorizing agents-in some embodiments, a mixture of decolorizing agents containing activated clay and one or more decolorizing agents selected from the group consisting of diatomaceous earth, magnesium silicate, activated carbon, and perlite is used. In some embodiments, the decolorizing agent of the present invention is a mixture of activated clay and diatomaceous earth, with particle size ranging from 0.1 to 100 microns, median particle size ranging from 10 to 20 μm, and a deviation value of the particle size distribution ranging from-0.3 to-0.7; or a mixture of activated clay and magnesium silicate, the particle size range is 0.1-100 microns, the median particle size range is 8-30 microns, and the deviation value of the particle size distribution is-0.3-0.9; or a mixture of activated clay and activated carbon, the particle size range is 0.1-100 microns, the median particle size range is 3-10 microns, and the deviation value of the particle size distribution is-0.5-0.9; or perlite with the particle size range of 0.1-100 microns, the median particle size range of 3-10 microns and the deviation value of particle size distribution of-0.3-0.6; or a mixture of perlite and active carbon, the particle size range is 0.1-100 microns, the median particle size range is 20-30 microns, and the deviation value of particle size distribution is-0.5-0.9; or a mixture of magnesium silicate and diatomite, the particle size range is 0.1-100 microns, the median particle size range is 20-30 microns, and the deviation value of the particle size distribution is-0.3-0.7; or the mixture of activated clay and perlite, the particle size range is 0.1-100 microns, the median particle size range is 3-10 microns, and the deviation value of the particle size distribution is-0.3-0.6; or activated clay with the particle size range of 0.1-100 microns, the median particle size range of 3-30 microns and the deviation value of particle size distribution of-0.5-0.9.
Generally, in the grease decoloring method, the usage amount of the decoloring agent is 1-5%, preferably 2-4% of the weight of the grease. The temperature and time of decolorization are not particularly limited, and can be determined by conventional means depending on the kind of the specific crude oil, the kind of the decolorizer used, and the amount of the decolorizer. An exemplary decolorization temperature is 100-.
Oils suitable for use in the oil decolorization process of the present invention are particularly those oils for which improved freezing resistance is desired, including but not limited to rice oil, cottonseed oil, soybean oil, sunflower oil, corn oil, or any mixture thereof.
In some embodiments of the present invention, it has been found that the oil or fat to be decolorized according to the present invention may not be dewaxed in advance by using the method of the present invention, i.e., the oil or fat to be decolorized according to the present invention may not be dewaxed in advance. The invention discovers that the method can greatly reduce energy consumption, greatly prolong the freezing time of the grease and obviously improve the freezing resistance. In some embodiments, dewaxing may be performed first, and then decolorization may be performed, which also greatly prolongs the freezing time of the grease, significantly improving freezing resistance.
In some embodiments, the present invention provides a method of refining fats and oils, comprising a step of decolorizing fats and oils as described herein and one or more steps selected from degumming, deacidification, neutralization, degreasing, deodorization. It is to be understood that one or more of the degumming, deacidification, neutralization, degreasing/dewaxing, and deodorization may be omitted depending on the actual production conditions and the purpose of the production. The process conditions of degumming, deacidification, neutralization, degreasing and deodorization can be conventional in the field and are adjusted according to the actual production conditions.
Exemplary degumming includes filtering the crude oil to remove solid impurities and adding a degumming medium to degum the crude oil. The degumming medium may be a degumming medium conventional in the art, such as citric acid solution, phosphoric acid solution and degumming enzyme. When using degumming enzymes such as PLA1 phospholipase, the reaction system is generally at 45-80 deg.C, pH 5-6, and time 2-6 h. The degumming medium is not less than 0.05 wt% of the weight of the crude oil, and is usually not more than 2 wt% of the weight of the crude oil. When an acid is used, the concentration of the acid is not less than 5 wt%, usually not more than 80 wt%, for example, it may be in the range of 5 to 65 wt%, 10 to 60 wt%, 20 to 50 wt%, based on the total weight of the solution. Water may be added simultaneously, usually in an amount of not less than 0.5% by weight based on the weight of the crude oil; typically, the amount of water used in a single degumming step is not more than 30 wt% of the oil weight, e.g. in the range of 0.5 to 20 wt%, 0.5 to 10 wt%, 5 to 25 wt%, excluding the water in the degumming medium. And separating the colloid after the reaction is finished to obtain the degummed oil.
In some embodiments, the crude oil is degummed by using PLA1 phospholipase, the addition mass of the phospholipase is 10-1000mg/kg of the mass of the crude oil, the reaction temperature is 45-50 ℃, the reaction time is 4-6h, the reaction pH value is 5-5.3, and after the reaction is finished, colloid is separated to obtain degummed oil.
In some embodiments, dewaxing is performed after degumming. An exemplary dewaxing process includes pumping degummed oil into a seed tank, controlling the temperature to 48-55 deg.C, and after a period of stabilization, e.g., 20-40 minutes, cooling to crystallize. Reducing the temperature to about 20 ℃ within 55-65 hours, growing the crystal at the temperature for 3-8 hours, and filtering after the crystal growth is finished.
The main purpose of deacidification is to remove free fatty acids from the crude oil and to remove some impurities such as pigments, phospholipids, hydrocarbons and mucilage. Physical deacidification methods may be used for deacidification. For example, the degummed oil may be treated at a pressure of 0.02 to 0.6kPa and a temperature of 180 ℃ and 250 ℃ to obtain a deacidified oil. Alternatively, deacidification may be carried out by an alkali refining process. For example, adding a proper amount of alkali liquor into the degummed oil at 80-90 ℃ for reaction for 10-60 minutes. Usually, the amount of alkali added is 7.13X 10-4×MOilX AV x (1+ excess alkali), the excess alkali can be 0-20%, the alkali liquor amount is alkali adding amount/alkali liquor concentration, wherein, MOilOil weight, AV acid number. Inverse directionAnd centrifuging after finishing reaction to obtain the neutralized oil.
If the deacidification is carried out by adopting an alkali refining mode, the alkali refined oil (neutralized oil) can be washed and dried firstly to carry out the soaping, and the soaped oil is obtained. For example, the neutralized oil can be heated to 80-90 deg.C, washed with hot water at a weight of less than 5 wt% (e.g., 1-3 wt%) of the oil, centrifuged, and vacuum dried at 90-120 deg.C to obtain the desaponified oil. It is understood that physical deacidification may be followed by caustic refining, if desired.
It is understood that deacidification may be done before decolorization or after decolorization, but before defatting.
An exemplary degreasing/dewaxing process comprises pumping the oil to be degreased into a crystal growing tank, controlling the temperature to 50-60 ℃, standing for 10-60min, and then cooling and crystallizing. Reducing the temperature to 0-6 ℃ within 10-60 hours, then growing the crystal at the temperature for 6-10 hours, and filtering after the crystal growth is finished.
An exemplary deodorization process comprises deodorizing at a vacuum of 25mbar or less at 180 ℃ and 240 ℃ for 30-150 minutes. The deodorization can be carried out in a deodorizing medium such as nitrogen.
In some embodiments, the invention includes a method of refining fats and oils comprising the steps of degumming, decolorizing, physical deacidification, neutralization, water washing drying and degreasing as described herein in sequence; in some embodiments, the oil and fat refining process of the present invention comprises the steps of degumming, neutralization, water wash drying, decolorization, degreasing, and optionally deodorization as described herein, in that order. In some embodiments, the oil refining process of the present invention comprises, in order, degumming, dewaxing, decolorizing, physical deacidification, neutralization, water wash drying, and degreasing steps. In some embodiments, the oil and fat refining process of the present invention comprises, in order, degumming, neutralization, water wash drying, decolorization, dewaxing, and optionally a deodorization step.
The invention also comprises the decolored grease obtained by the decoloration method, the refined grease obtained by the refining method and blend oil containing the refined grease. Preferably, the oil is rice oil, cottonseed oil, soybean oil, sunflower seed oil, corn oil or any mixture thereof.
The invention also provides the application of the decolorizing agent with the particle size distribution range of 0.1-100 microns, the median particle size range of 1-30 microns and the deviation value of the particle size distribution of-0.3-1 in improving the oil freezing time; preferred depigmenting agents are as described in any of the embodiments herein.
The decoloring agent containing at least two of activated clay, diatomite, magnesium silicate, activated carbon and perlite is also in the scope of the invention, and is characterized in that the particle size distribution range of all particles of the decoloring agent is 0.1-100 microns, the median particle size range is 1-30 microns, and the deviation value of the particle size distribution is-0.3-1. Preferred examples of such decolorizing agents are as described in any of the decolorizing agent mixture embodiments herein.
The present invention will be illustrated below by way of specific examples. It is to be understood that these examples are illustrative only and are not intended to limit the scope of the present invention.
Sources of decolorizing agents used in the examples:
clay: specification of clean bleaching earth ltd, le ping city: 1020 #.
Activated carbon: a bajiali wood plant of the sea of Yi.
Diatomite: specification of diatomite new material Limited company in Yangtze Shangjin: the earth brand diatomite filter aid.
Perlite: filtration aid limited, zhongnan, province, he, specification: saussurea involucrate brand GK-110
Magnesium silicate: dallas (Qingdao) Special adsorbents, Inc
The following methods were used in the examples:
1. freezing experiment
With reference to GB/T17756, the method of operation is as follows:
1) heating the uniformly mixed finished oil sample (200-300 mL) to 130 ℃, immediately stopping heating, and filtering while the sample is hot;
2) injecting the filtered oil into an oil sample bottle, plugging the bottle with a cork, cooling to 25 ℃, and sealing with paraffin;
3) the oil bottle was then immersed in an ice-water bath at 0 ℃ and the timer was started. Covering with ice water, and keeping the ice water bath at 0 ℃;
4) the sample was recorded for haziness or crystallization or precipitation time.
2. Yield of the product
The yield of the finished oil is 100% of the quality of the finished oil/the quality of the crude oil.
3. Electricity consumption
The power consumption of each ton of oil is kW.h/T.
4. Median particle size and particle size distribution range
Median particle diameter (Md): refers to the corresponding particle size in millimeters (or phi values) at a particle content of 50% on the cumulative curve. The test was carried out using an LS13320 laser particle sizer (dry module). The particle size distribution range of the sample is also detected by an LS13320 laser particle size analyzer (dry module).
5. Deviation value
The deviation value (SK1) is a parameter used to represent the symmetry of the frequency curve, and substantially reflects the degree of asymmetry of the particle size distribution. Detection was performed using an LS13320 laser particle sizer (dry module). And calculating according to the detection result. The calculation formula is as follows:
Figure BDA0002350923060000091
comparative example 1
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the addition amount of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. dewaxing: pumping the degummed oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 20 ℃ within 60 hours, growing the crystal for 5 hours at the temperature of 20 ℃, and filtering after the crystal growing is finished;
3. and (3) decoloring: adding activated clay with the mass of 2% of the degummed rice oil, wherein the particle size range is 100-150 mu m, the median particle size is 120 mu m, the deviation value of the particle size distribution is 0, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
4. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and deacidifying rice oil is obtained after 2h of reaction;
5. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 0.5% of that of the oil, reacting for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
6. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
7. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Comparative example 2
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay with the mass of 2% of the degummed rice oil, wherein the particle size range is 100-150 mu m, the median particle size is 120 mu m, the deviation value of the particle size distribution is 0, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and deacidifying rice oil is obtained after 2h of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Comparative example 3
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay and diatomite with the mass of 2% of the degummed rice oil, wherein the particle size range is 150 mu m, the median particle size is 120 mu m, the deviation value of the particle size distribution is-0.7, and reacting for 30min at the temperature of 115 ℃ under the pressure of 6kPa to obtain destaining oil; (ii) a
3. Physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and reacting for 2 hours to obtain deacidified rice oil;
4. neutralizing: and (3) cooling the deacidified oil obtained in the previous step to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil, reacting for 30min, and centrifuging after the reaction is finished to obtain the neutralized oil. (ii) a
5. Washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain the final product. (ii) a
6. Degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Comparative example 4
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay and diatomite with the mass of 2% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 75 μm, the deviation value of the particle size distribution is-0.7, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destaining oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Comparative example 5
1. Method for preparing grease
1. Degumming: filtering crude cottonseed oil to remove solid impurities, adding a phosphoric acid aqueous solution (concentration is 10%) with the weight of 0.2% of that of the oil, heating to 60 ℃, reacting for 30min, and separating colloid to obtain degummed oil;
2. neutralizing: controlling the temperature of the degummed oil obtained in the previous step to 80 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of the oil to react for 30min, and centrifuging after the reaction is finished to obtain neutralized oil 3. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
4. and (3) decoloring: adding perlite and active carbon with a particle size range of 0.1-100 μm and a median particle size of 70 μm in an amount of 2% by mass of desoponated cottonseed oil, reacting at 115 deg.C under 6kPa for 30min to obtain decolorized oil;
5. degreasing: pumping deodorized oleum gossypii into crystal growth tank, controlling temperature to 50 deg.C, stabilizing for 30min, and cooling for crystallization. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
6. Deodorizing: deodorizing decolorized oleum gossypii semen at 210 deg.C under vacuum degree of 10mbar for 2 hr to obtain deodorized oleum gossypii semen.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Comparative example 6
1. Method for preparing grease
1. Degumming: filtering crude corn oil to remove solid impurities, adding a phosphoric acid aqueous solution (the concentration is 10%) with the weight of 0.1% of that of the oil, heating to 60 ℃, reacting for 30min, and separating colloid to obtain degummed oil;
2. neutralizing: controlling the temperature of the degummed oil obtained in the previous step to 80 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil.
3. Washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
4. and (3) decoloring: adding argil with a particle size range of 0.1-100 μm and a median particle size of 70 μm in an amount of 2% by mass of the saponified corn oil, reacting at 115 ℃ under 6kPa for 30min under a deviation value of-0.5 in particle size distribution to obtain decolorized oil;
5. dewaxing: pumping the decolorized corn oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 6 ℃ within 15 hours, growing the crystal for 6 hours at the temperature of 6 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
6. Deodorizing: deodorizing the dewaxed corn oil at 210 deg.C under vacuum degree of 10mbar for 2h to obtain deodorized corn oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Comparative example 7
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
3. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
4. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
5. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
6. And (3) decoloring: adding activated clay and diatomite with the mass of 2% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 15 μm, the deviation value of the particle size distribution is-0.5, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destaining oil;
7. deodorizing: deodorizing the decolorized oil at 240 deg.C under vacuum degree of 10mbar for 2 hr to obtain deodorized oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 1
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay and diatomite with the mass of 2% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 15 μm, the deviation value of the particle size distribution is-0.5, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destaining oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 2
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay and magnesium silicate with the mass of 2.5% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 25 μm, the deviation value of the particle size distribution is-0.5, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destaining oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 3
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay and activated carbon with the mass of 2% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 5 μm, the deviation value of the particle size distribution is-0.7, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 4
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding perlite with the mass of 2% of the degummed rice oil, the particle size range of 0.1-100 μm, the median particle size of 5 μm, the deviation value of the particle size distribution of-0.4, and reacting at 115 ℃ under the pressure of 6kPa for 30min to obtain destaining oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (the concentration is 10%) with the weight of 5% of the oil, reacting for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 5
2. Method for preparing grease
1. Degumming: filtering crude cottonseed oil to remove solid impurities, adding a phosphoric acid aqueous solution (concentration is 10%) with the weight of 0.2% of that of the oil, heating to 60 ℃, reacting for 30min, and separating colloid to obtain degummed oil;
2. neutralizing: controlling the temperature of the degummed oil obtained in the previous step to 80 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of the oil to react for 30min, and centrifuging after the reaction is finished to obtain neutralized oil 3. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
4. and (3) decoloring: adding perlite and active carbon with a particle size range of 0.1-100 μm and a median particle size of 25 μm in an amount of 2% by mass of desoponated cottonseed oil, reacting at 115 deg.C under 6kPa for 30min to obtain decolorized oil, wherein the particle size distribution deviation is-0.6;
5. degreasing: pumping deodorized oleum gossypii into crystal growth tank, controlling temperature to 50 deg.C, stabilizing for 30min, and cooling for crystallization. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
6. Deodorizing: deodorizing decolorized oleum gossypii semen at 210 deg.C under vacuum degree of 10mbar for 2 hr to obtain deodorized oleum gossypii semen.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 6
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding magnesium silicate and diatomite with a particle size range of 0.1-100 μm and a median particle size of 30 μm, wherein the mass of the degummed rice oil is 2%, reacting at 115 ℃ under 6kPa for 30min to obtain decolorized oil, wherein the deviation value of the particle size distribution is-0.5;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circular treatment, wherein the system pressure is 0.3kPa and the temperature is 220 ℃, and obtaining the fine deacidified rice oil;
4. neutralizing: cooling the deacidified oil to 50 deg.C, adding 5 wt% sodium hydroxide water solution (concentration of 10%) for reaction for 30min, and centrifuging to obtain neutralized oil
5. Washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 7
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding perlite and activated clay with the mass of 2% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 3 μm, the deviation value of the particle size distribution is-0.3, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain decolorized oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and deacidifying rice oil is obtained after 2h of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 8
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay and magnesium silicate with the mass of 3% of the degummed rice oil, the particle size range is 0.1-100 μm, the median particle size is 10 μm, the deviation value of the particle size distribution is-0.9, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and deacidifying rice oil is obtained after 2h of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 9
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the addition amount of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. dewaxing: pumping the degummed oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 20 ℃ within 60 hours, growing the crystal for 5 hours at the temperature of 20 ℃, and filtering after the crystal growing is finished;
3. and (3) decoloring: adding activated clay with the mass of 2% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 5 μm, the deviation value of the particle size distribution is-0.8, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
4. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and the deacidified rice oil is obtained after 2 hours of reaction;
5. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 0.5% of that of the oil, reacting for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
6. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
7. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 10
1. Method for preparing grease
1. Degumming: filtering crude corn oil to remove solid impurities, adding a phosphoric acid aqueous solution (the concentration is 10%) with the weight of 0.1% of that of the oil, heating to 60 ℃, reacting for 30min, and separating colloid to obtain degummed oil;
2. neutralizing: controlling the temperature of the degummed oil obtained in the previous step to 80 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil.
3. Washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
4. and (3) decoloring: adding activated clay with particle size of 0.1-100 μm and median particle size of 25 μm in an amount of 2% of the weight of the saponified corn oil, reacting at 115 deg.C under 6kPa for 30min to obtain decolorized oil, wherein the particle size distribution deviation is-0.6;
5. dewaxing: pumping the decolorized corn oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 6 ℃ within 15 hours, growing the crystal for 6 hours at the temperature of 6 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
6. Deodorizing: deodorizing the dewaxed corn oil at 210 deg.C under vacuum degree of 10mbar for 2h to obtain deodorized corn oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 11
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay with the mass of 1% of the degummed rice oil, wherein the particle size range is 0.1-100 μm, the median particle size is 10 μm, the deviation value of the particle size distribution is-0.9, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and deacidifying rice oil is obtained after 2h of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
Example 12
1. Method for preparing grease
1. Degumming: filtering rice crude oil to remove solid impurities, degumming the crude oil by using PLA1 phospholipase, wherein the added mass of the phospholipase is 100mg/kg of the mass of the crude oil, the reaction temperature is 45 ℃, the reaction time is 4h, the reaction pH value is 5, and after the reaction is finished, separating colloid to obtain degummed oil;
2. and (3) decoloring: adding activated clay with 5% of the degummed rice oil, the particle size range is 0.1-100 μm, the median particle size is 10 μm, the deviation value of the particle size distribution is-0.9, and reacting for 30min at 115 ℃ under the pressure of 6kPa to obtain destained oil;
3. physical deacidification: pumping the decolorized oil obtained in the previous step into a falling film evaporator for circulation treatment, wherein the system pressure is 0.3kPa, the temperature is 220 ℃, and deacidifying rice oil is obtained after 2h of reaction;
4. neutralizing: cooling the deacidified oil to 50 ℃, adding a sodium hydroxide aqueous solution (with the concentration of 10%) with the weight of 5% of the oil for reaction for 30min, and centrifuging after the reaction is finished to obtain neutralized oil;
5. washing and drying: heating the neutralized oil to 80 deg.C, adding soft water 3% of the oil weight, washing with water, centrifuging, and vacuum drying at 110 deg.C to obtain soapless oil;
6. degreasing: pumping the desquamated oil into a crystal growing tank, controlling the temperature to 50 ℃, stabilizing for 30min, and beginning to cool and crystallize. Reducing the temperature to 4 ℃ within 60 hours, growing the crystal for 10 hours at the temperature of 4 ℃, and filtering after the crystal growing is finished to obtain the finished oil.
2. Freezing experiment
The freezing test was conducted as described above, and the freezing-resistant time of the rice oil was measured after the completion of the freezing test. The results of the experiment are shown in table 1.
3. Yield and power consumption
The yield and power consumption were calculated as described above. The results of the experiment are shown in table 1.
TABLE 1
Figure BDA0002350923060000261
Figure BDA0002350923060000271
Note: the particle size ranges and median particle sizes are reported in microns.

Claims (10)

1. The method for decoloring the grease is characterized by decoloring the grease to be decolored by using a decoloring agent with a particle size distribution range of 0.1-100 microns, a median particle size range of 1-30 microns and a deviation value of particle size distribution of-0.3-1.
2. A method of decoloring fats and oils according to claim 1,
the decolorizing agent is selected from activated clay, attapulgite, zeolite, acidified rice hull ash, magnesium silicate, diatomite, perlite, activated carbon and any mixture thereof; preferably, the decolorant is activated clay, perlite, a mixture of perlite and activated carbon, a mixture of magnesium silicate and diatomite, and a mixture of activated clay and other decolorants; preferably, the decolorizing agent comprises a mixture of activated clay and one or more decolorizing agents selected from diatomaceous earth, magnesium silicate, activated carbon and perlite; and/or
The oil is oil which needs to improve the freezing resistance, and is preferably rice oil, cottonseed oil, soybean oil, sunflower seed oil, corn oil or any mixture thereof; preferably, the oil or fat to be decolorized has not been subjected to dewaxing treatment.
3. A method of decoloring fats and oils according to claim 1,
the median particle size range of the decolorizing agent is 3-30 mu m, preferably 5-15 mu m;
the deviation value of the particle size distribution of the decolorizing agent is-0.3 to-0.9, preferably-0.5 to-0.9, and more preferably-0.7 to-0.9; and/or
The usage amount of the decolorizing agent is 1-5% of the weight of the oil, and preferably 2-4%.
4. A method of decoloring fats and oils according to claim 1,
the decolorizing agent is a mixture of activated clay and diatomite, the particle size range is 0.1-100 micrometers, the median particle size range is 10-20 micrometers, and the deviation value of particle size distribution is-0.3-0.7;
the decolorizing agent is a mixture of activated clay and magnesium silicate, the particle size range is 0.1-100 microns, the median particle size range is 8-30 microns, and the deviation value of particle size distribution is-0.3-0.9;
the decolorizing agent is a mixture of activated clay and activated carbon, the particle size range is 0.1-100 microns, the median particle size range is 3-10 microns, and the deviation value of particle size distribution is-0.5-0.9;
the decolorizing agent is perlite, the particle size range is 0.1-100 microns, the median particle size range is 3-10 microns, and the deviation value of particle size distribution is-0.3-0.6;
the decolorizing agent is a mixture of perlite and activated carbon, the particle size range is 0.1-100 microns, the median particle size range is 20-30 microns, and the deviation value of particle size distribution is-0.5-0.9;
the decolorizing agent is a mixture of magnesium silicate and diatomite, the particle size range is 0.1-100 micrometers, the median particle size range is 20-30 micrometers, and the deviation value of particle size distribution is-0.3-0.7;
the decolorizing agent is a mixture of activated clay and perlite, the particle size range is 0.1-100 microns, the median particle size range is 3-10 microns, and the deviation value of particle size distribution is-0.3-0.6; or
The decolorizing agent is activated clay, the particle size range is 0.1-100 microns, the median particle size range is 3-30 microns, and the deviation value of particle size distribution is-0.5-0.9.
5. The method for decoloring oil and fat according to claim 1, wherein the decoloring is performed at a temperature of 100-120 ℃ and the decoloring time is 10-60 minutes.
6. A method for refining oil, wherein the oil is decolorized by the oil decolorization method according to any one of claims 1 to 5 before dewaxing and/or degreasing, and preferably the method further comprises one or more steps of degumming, deacidification, neutralization and deodorization.
7. A decoloring agent with a particle size distribution range of 0.1-100 microns, a median particle size range of 1-30 microns and a deviation value of the particle size distribution of-0.3-1, or the application of the oil decoloring method according to any one of claims 1-5 in improving the oil freezing time; preferably, the depigmenting agent is as claimed in any one of claims 2 to 4.
8. The decoloring agent is characterized by comprising at least two of activated clay, diatomite, magnesium silicate, activated carbon and perlite, wherein the particle size distribution range of the decoloring agent particles is 0.1-100 microns, the median particle size range is 1-30 microns, and the deviation value of the particle size distribution is-0.3-1.
9. The decolorizing agent of claim 8, wherein the decolorizing agent is:
the mixture of the activated clay and the diatomite has the particle size range of 0.1-100 microns, the median particle size range of 10-20 microns and the deviation value of particle size distribution of-0.3-0.7;
a mixture of activated clay and magnesium silicate, wherein the particle size range is 0.1-100 microns, the median particle size range is 8-30 microns, and the deviation value of particle size distribution is-0.3-0.9;
the mixture of activated clay and activated carbon has the particle size range of 0.1-100 microns, the median particle size range of 3-10 microns and the deviation value of particle size distribution of-0.5-0.9;
the mixture of perlite and active carbon has a particle size range of 0.1-100 microns, a median particle size range of 20-30 microns and a deviation value of particle size distribution of-0.5-0.9;
a mixture of magnesium silicate and diatomite, wherein the particle size range is 0.1-100 microns, the median particle size range is 20-30 microns, and the deviation value of particle size distribution is-0.3-0.7; or
The mixture of the activated clay and the perlite has the particle size range of 0.1-100 microns, the median particle size range of 3-10 microns and the deviation value of particle size distribution of-0.3-0.6.
10. A fat or oil produced by the method according to any one of claims 1 to 6.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017039840A (en) * 2015-08-19 2017-02-23 日清オイリオグループ株式会社 Process for producing purified oil/fat
JP2017088414A (en) * 2015-11-02 2017-05-25 水澤化学工業株式会社 Decolorant, and method for producing decolorant

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017039840A (en) * 2015-08-19 2017-02-23 日清オイリオグループ株式会社 Process for producing purified oil/fat
JP2017088414A (en) * 2015-11-02 2017-05-25 水澤化学工業株式会社 Decolorant, and method for producing decolorant

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
徐爱军: "一级大豆油抗冻 性影响因素的研究", 中国油脂, vol. 38, no. 1, pages 38 *
赵军: "影响油脂脱色效果的因素", 中国油脂, vol. 28, no. 2, pages 21 *

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