CN110835582A - Preparation method of grease with high retention of functional components and flavor - Google Patents
Preparation method of grease with high retention of functional components and flavor Download PDFInfo
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- CN110835582A CN110835582A CN201911152408.XA CN201911152408A CN110835582A CN 110835582 A CN110835582 A CN 110835582A CN 201911152408 A CN201911152408 A CN 201911152408A CN 110835582 A CN110835582 A CN 110835582A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
Abstract
A method for preparing oil with high retention of functional components and flavor comprises the following steps: (1) oil pretreatment, wherein the step can select one of hydration treatment and enzyme treatment; (2) modifying a tubular multi-channel ceramic membrane; (3) filtering by a ceramic membrane filter and (5) cleaning and storing by the ceramic membrane. The invention adopts an enzyme membrane combination method to prepare the high-retention nutrition and flavor grease. Can achieve high retention rate for functional components in oil such as vitamin E, sterol, unsaturated fatty acid, etc., and characteristic flavor substances of oil.
Description
Technical Field
The invention belongs to the technical field of oil processing, and relates to a preparation method of oil with high retention of functional components and flavor.
Background
With the improvement of scientific and technical level and life of people, people pursue more and more nutrition and fragrance of grease, and the country advocates green energy-saving technology. So that more and more emerging technologies are applied to the grease industry. Enzymatic degumming and membrane techniques are two of them. The enzymatic degumming utilizes the unique high-efficiency hydrolysis catalytic capability of phospholipase on phospholipid to convert non-hydrated phospholipid into hydrated phospholipid so as to separate the non-hydrated phospholipid from the oil. The membrane technology is a technology for separating, purifying and concentrating different components of feed liquid by utilizing selective separation of a membrane.
Grease is one of three major nutrients and is a substance which must be taken in life. In the life of people, the most common edible oil is vegetable oil. Common vegetable oils include: soybean oil, rapeseed oil and peanut oil, corn oil, tea seed oil, and the like. These conventional virgin vegetable oils have their unique flavors and abundant nutrients, but not only much flavor and nutrients are lost due to excessive refining and excessive refining steps, but their unique flavors are hardly heard even in the finished oils and functional ingredients are almost lost. With the discharge of aromatic grease and the standard thereof, people are more and more pursuing functionality and flavor. Therefore, the elimination of unnecessary refining steps and the use of modest, green, energy-saving techniques on the necessary steps are an epoch's trend.
Different fats and oils have different characteristic flavors for their characteristic flavors. The oil material can present a plurality of different flavor substances in the thick fragrant oil obtained by pressing after frying. The source of the flavor substances mainly comprises 3 types of sources, namely (1) Maillard reaction between amino acid and sugar; (2) oxidation reaction of fat; (3) and (4) sugar degradation reaction. Wherein, Maillard reaction is an important way for generating flavor substances in the food processing process, and products mainly comprise nitrogen-oxygen heterocyclic compounds, such as pyrazine pyrrole pyridine compounds and the like; the oxidation reaction of fat is an inevitable reaction for generating flavor in the hot pressing process of oil materials, and main products of the oxidation reaction are acid, aldehyde, ketone, hydrocarbon compounds and the like; the sugar degradation reaction can form carbonyl, olefin, acid, furan and pyran compounds.
Disclosure of Invention
The invention aims to provide a method for preparing oil with high retention of functional components and flavor.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: a method for preparing grease with high retention of functional components and flavor,
the filter element of the ceramic membrane filter is a modified tubular multi-channel ceramic membrane;
the method for modifying the modified tubular multi-channel ceramic membrane comprises the following steps: soaking the tubular multi-channel ceramic membrane in pure water for 12-24 hours, drying the tubular multi-channel ceramic membrane in an oven for more than 6 hours, and filling the tubular multi-channel ceramic membrane into a ceramic membrane component to form a ceramic membrane filter; dissolving an organosilane coupling agent in absolute ethyl alcohol, and stirring for 30-60 minutes to obtain an ethanol solution of the organosilane coupling agent;
preheating the tubular multi-channel ceramic membrane to above 80 ℃, heating and gasifying an ethanol solution of the organosilane coupling agent, and then contacting the coupling agent with the tubular multi-channel ceramic membrane to modify the tubular multi-channel ceramic membrane to obtain a modified tubular multi-channel ceramic membrane;
the preparation method comprises the following steps:
step 1: pretreating the crude oil to obtain pretreated crude oil; the pretreatment adopts one of the following two oil pretreatment methods:
the pretreatment method comprises the following steps: filtering the crude oil, heating to 60-80 deg.C, adding 60-80 deg.C hot water 0.3-0.5% of crude oil weight, stirring, standing at 60-80 deg.C for 3-5 hr to complete hydration;
and a second pretreatment method: preheating crude oil at 60-80 deg.C, adding citric acid buffer solution 15-25mL per kg crude oil, homogenizing, and stirring for 10-20 min; cooling to 40-55 deg.C, adding enzymatic reaction catalyst 0.4-0.6% of crude oil, homogenizing, and degumming in 40-55 deg.C water bath under stirring for 2-4 hr; after the reaction is finished, if the enzymatic reaction catalyst contains free phospholipase, heating to inactivate the enzyme, and if immobilized enzyme is adopted, recovering the immobilized enzyme; the enzymatic reaction catalyst is formed by mixing distilled water with at least one of protease and phospholipase;
step 2: connecting a plurality of ceramic membrane filters in series, and then filtering the pretreated crude oil, wherein the filtering pressure is 0.05-1 Mpa, the temperature is 20-80 ℃, and the membrane surface flow rate is 1-6 m/s; the pretreated crude oil is pumped into a first-stage ceramic membrane filter, clean oil permeates the first-stage ceramic membrane filter under the pressure drive and is collected into a ceramic membrane clear liquid tank, concentrated solution obtained by the first-stage ceramic membrane filter is sent into a second-stage ceramic membrane filter as raw material, the clean oil permeates a second-stage ceramic membrane under the pressure drive and is collected into the ceramic membrane clear liquid tank, concentrated solution obtained by the second-stage ceramic membrane filter is sent into a third-stage ceramic membrane filter as raw material, the clean oil permeates the third-stage ceramic membrane filter under the pressure drive and is collected into the ceramic membrane clear liquid tank, and the rest is done by analogy, and concentrated solution obtained by the last-stage ceramic membrane filter enters the ceramic membrane concentrated liquid tank;
and step 3: feeding the concentrated solution obtained by the last stage of ceramic membrane filter stored in the ceramic membrane concentrated solution tank into a centrifuge for centrifugal separation; returning the obtained clear liquid to the ceramic membrane raw material tank, and continuously filtering; returning the thick slag of the centrifuge to the squeezing section.
The preferable technical scheme is as follows: the tubular multi-channel ceramic membrane is formed by sintering at least one material of alumina, zirconia, titania and silica at high temperature; the aperture of the tubular multi-channel ceramic membrane is 0.02-0.5 microns.
The preferable technical scheme is as follows: the homogenizing treatment rate is 10000-20000 r/min, and the treatment time is 0.5-1.5 min.
The preferable technical scheme is as follows: the protease is free protease or immobilized protease; the phospholipase is free phospholipase or immobilized phospholipase.
The preferable technical scheme is as follows: the device also comprises a device for modifying the tubular multi-channel ceramic membrane: the outlet of the ceramic membrane filter is communicated with an air inlet pipe of a vacuum pumping system through a first pipeline; the inlet of the ceramic membrane filter is communicated with the air outlet of an air heating system through a second pipeline, and the path of the second pipeline is communicated with a storage tank for storing ethanol solution of the organosilane coupling agent through a third pipeline.
The preferable technical scheme is as follows: the crude oil is at least one of hot pressed rapeseed oil, soybean oil, peanut oil, corn germ oil, cottonseed oil, rice bran oil, sunflower seed oil, tea seed oil and other vegetable oil crude oil, and the phospholipid content is 80-400 mg/kg.
The preferable technical scheme is as follows: before the ceramic membrane filter is used, firstly, baking the modified tubular multichannel ceramic membrane in a baking oven at 70 ℃ for 1h, then, carrying out oil rinsing on the tubular multichannel ceramic membrane by adopting refined first-level, second-level, third-level and fourth-level grease at the pressure difference of 0.1-0.8 Mpa, the temperature of 20-80 ℃ and the flow rate of 1-6 m/s so as to stabilize the performance of the tubular multichannel ceramic membrane; the oil is rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, rice bran oil, sunflower seed oil or tea seed oil.
The preferable technical scheme is as follows: filtering the pretreated crude oil by using a vertical leaf filter or a metal pipe network filter; the filtration precision is 10-500 meshes, and the filtration pressure is 0.05-1 Mpa.
The preferable technical scheme is as follows: cleaning solution adopted by the tubular multi-channel ceramic membrane is refined first-level, second-level, third-level and fourth-level grease; the oil is rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, rice bran oil, sunflower seed oil or tea seed oil; the cleaning method comprises the following steps: adding 8-12 liters of cleaning solution into the ceramic membrane filter, starting the ceramic membrane filter, and carrying out reflux operation for 30-60min under the conditions that: the membrane pressure difference is 0.1-0.3 Mpa, the temperature is 25-60 ℃, and the flow rate is 1-6 m/s; the operation is repeated at least once.
Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:
the invention adopts an enzyme membrane combination method to prepare the high-retention nutrition and flavor grease. Can achieve high retention rate for functional components in oil such as vitamin E, sterol, unsaturated fatty acid, etc., and characteristic flavor substances of oil.
Drawings
FIG. 1 is a schematic diagram of an apparatus for modifying a tubular multi-channel ceramic membrane.
In the above figures, 1, a ceramic membrane filter; 2. a vacuum pumping system; 3. an air heating system; 4. and (4) storage tank.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Please refer to fig. 1. It should be understood that the structures, ratios, sizes, and the like shown in the drawings and described in the specification are only used for matching with the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented, so that the present invention has no technical significance, and any structural modification, ratio relationship change, or size adjustment should still fall within the scope of the present invention without affecting the efficacy and the achievable purpose of the present invention. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
Example 1: preparation method of grease with high retention of functional components and flavor
The preparation method of the aromatic oil by the enzyme membrane method is characterized by comprising the following steps.
(1) Pretreatment of oil
The oil is one or more of hot pressed crude vegetable oil such as rapeseed oil, soybean oil, peanut oil, corn germ oil, cottonseed oil, rice bran oil, sunflower seed oil and tea seed oil, and the phospholipid content is (80-400 mg/kg). This example is rapeseed oil, and the phospholipid content was found to be 235 mg/kg.
1) Hydration treatment: rapeseed oil crude oil was filtered, heated to 70 ℃ oil temperature, then added with 70 ℃ hot water in an amount of 0.5% by weight of the crude oil, stirred to mix well, slightly raised in temperature, and allowed to settle in a container at about 71 ℃ for 4h to complete hydration.
2) Enzyme treatment:
preheating rapeseed oil crude oil at 70 deg.C for 10min, adding 20mL citric acid buffer solution with pH of 7.0 per kg oil, homogenizing at 10000r/min for 1 min, and processing with digital display stirrer 500 r/min for 15 min. And (2) reducing the temperature to 45 ℃, adding an enzymatic reaction catalyst accounting for 0.5 percent of the mass of the crude rapeseed oil, wherein the enzymatic reaction catalyst is prepared by mixing distilled water and protease according to a ratio of 95: 1 in mass ratio. Homogenizing at 1000 r/min for 1 min, and degumming at 45 deg.C in a water bath at 500 r/min for 3 h. After the reaction is finished, enzyme in the degummed oil is inactivated by water bath for 10min at the temperature of 90 ℃.
(2) Ceramic membrane plant treatment
1) Ceramic membranes used for illustration
The ceramic membrane is a tubular multi-channel ceramic membrane and is prepared by sintering alumina and zirconia at high temperature. The preparation method of the tubular multi-channel ceramic membrane is the prior art.
The aperture of the tubular multi-channel ceramic membrane is 0.02-0.5 micron.
The ceramic membrane has a hydrophobic surface.
The hydrophobic ceramic membrane is prepared by chemical grafting modification by adopting an organosilane coupling agent, and the modification method is a gas phase method. Soaking the ceramic membrane in pure water for 18 hours, drying the ceramic membrane in an oven at 120 ℃ for 7 hours, and filling the ceramic membrane into a ceramic membrane module for later use. Dissolving the organosilane coupling agent in absolute ethyl alcohol, and stirring and reacting for 45 minutes for later use.
The heating system is connected with the membrane component, and the outlet of the membrane component is connected with the vacuum system. The whole system is preheated to more than 80 ℃, the ethanol solution is gradually injected into a heating system for gasification, the coupling agent is contacted and reacted with the ceramic membrane through a vacuum system, unreacted ethanol and the coupling agent are discharged through the vacuum system, and the modified ceramic membrane can be directly used after being simply dried for 1 hour at 120 ℃.
2) Illustrating the composition of the ceramic membrane equipment; the ceramic membrane equipment comprises a feeding pump, a circulating pump, a ceramic membrane support, a ceramic membrane assembly, a ceramic membrane filter element, an automatic control valve, pressure, temperature and flow sensors, a ceramic membrane control system and other core components. The ceramic membrane control system can receive parameters such as temperature, pressure, membrane surface flow rate and the like of system operation through temperature, pressure and flow sensors, and then control parameters such as valves of equipment, frequency converters of a feeding pump and a circulating pump and the like through an automatic control system, so as to control the parameters such as operating temperature, pressure, membrane surface flow rate and the like of ceramic membrane equipment and maintain the equipment to operate under stable temperature, pressure and membrane surface flow rate. The ceramic membrane equipment is designed to be operated by a plurality of sets of equipment in series, 2-10 stages can be connected in series, and parameters such as temperature, pressure, membrane surface flow velocity and the like of each stage are detected and controlled fully and automatically. The embodiment is specifically level 8, other accessories of the ceramic membrane equipment and the connection mode of the ceramic membrane equipment adopt the prior art, and the embodiment only carries out hydrophobic modification on the tubular multi-channel ceramic membrane in the prior art.
3) A pretreatment method is described that the ceramic membrane device needs to perform before being used for grease filtration.
If the ceramic membrane tube is used continuously until then, no treatment is required. If a new ceramic membrane tube is adopted, the membrane tube is firstly baked in an oven at 70 ℃ for 1h before filtration, and then refined first-level, second-level, third-level and fourth-level grease, such as rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, rice bran oil, sunflower seed oil and tea seed oil, or the membrane-filtered grease obtained in the technical scheme 2 is used for carrying out oil rinsing on the membrane tube under the pressure difference of 0.1Mpa-0.8Mpa, the temperature of 20-80 ℃ and the flow rate of 1m/s-6m/s so as to stabilize the performance of the membrane tube.
(3) Ceramic membrane tangent filtration parameter setting
Firstly, filtering the grease crude oil subjected to hydration and enzyme treatment by a vertical leaf filter or a metal pipe network filter before ceramic membrane filtration to remove large-particle suspended matters, wherein the filtering precision is 10-500 meshes, and the filtering pressure is 0.05-1 Mpa.
Then, according to different raw materials, the filtering aperture of the ceramic membrane can be selected to be 20-500 nm. The filtering pressure of the membrane equipment is 0.1-0.8 Mpa, the temperature is 20-80 ℃, and the flow rate of the membrane surface is 1-6 m/s. Crude oil of the grease after pretreatment, hydration, acidification and enzymatic treatment is sent to first-stage ceramic membrane equipment through a feeding pump, the crude oil is filtered by a ceramic membrane, impurities such as colloid and suspended matters are intercepted, and clean grease is collected to a ceramic membrane clear liquid tank through the first-stage ceramic membrane under the drive of pressure. And feeding the first-stage ceramic membrane concentrated solution serving as a raw material into second-stage ceramic membrane equipment, and collecting the clean grease into a ceramic membrane clear solution tank through a second-stage ceramic membrane under the drive of pressure. And feeding the second-stage ceramic membrane concentrated solution serving as a raw material into a third-stage ceramic membrane device, and collecting the clean grease into a ceramic membrane clear solution tank through a third-stage ceramic membrane under the drive of pressure. And by parity of reasoning, the ceramic membrane concentrated solution of the last stage enters a ceramic membrane concentrated solution tank.
4) Ceramic membrane concentrate treatment
And (4) feeding the ceramic membrane concentrated solution into a centrifugal machine for separation, and removing impurities such as colloid, suspended matters and the like. The centrifugation time is 5-30min, and the rotation speed is 4000-12000 rpm. Returning the obtained clear liquid of the centrifuge to the ceramic membrane raw material tank, continuously filtering, and returning the thick slag of the centrifuge to the squeezing working section.
(5) Ceramic membrane cleaning and preservation
1) The cleaning solution used for cleaning is refined first-grade, second-grade, third-grade and fourth-grade oils, such as rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, rice bran oil, sunflower seed oil, tea seed oil, or clear liquid oil obtained by membrane filtration in technical scheme 2.
2) Firstly, adding about 10 liters of cleaning fluid, starting the equipment, and carrying out reflux operation for 30-60min under the conditions that: the membrane pressure difference is 0.1-0.3 Mpa, the temperature is 25-60 ℃, and the flow rate is 1-6 m/s. Then, about 10 liters of the cleaning solution is replaced, the equipment is started, and the concentration operation is carried out for 30-60min under the same conditions.
Example 2: preparation method of grease with high retention of functional components and flavor
(1) Pretreatment of peanut crude oil: a certain amount of hot-pressed peanut crude oil is taken, and pretreatment can be carried out in two ways: 1) heating to oil temperature of about 65 deg.C, adding a certain amount of 65 deg.C hot water (0.5% of crude oil weight), stirring to mix thoroughly, slightly raising temperature, and standing in a reactor at about 65 deg.C for 3.5 h to complete hydration; 2) preheating at 65 deg.C for 10min, adding citric acid buffer solution 20mL per kg of oil, homogenizing at 12000 r/min for 1 min, and processing with digital display stirrer 500 r/min for 15 min. Cooling to 47 deg.C, adding 0.5% distilled water and phospholipase (mass ratio of distilled water to phospholipase is 10: 1) (such as single phospholipase A1, single phospholipase A2 and C or immobilized enzyme and mixture of phospholipase A1, phospholipase A2 and C or immobilized enzyme), homogenizing at 1000 r/min for 1 min, and degumming at 500 r/min in 47 deg.C water bath for 2.3 h. After the reaction is finished, if free phospholipase is adopted, enzyme in the degummed oil is inactivated in a water bath for 10min at the temperature of 90 ℃; if the immobilized enzyme is adopted, the immobilized enzyme is recovered.
(2) Ceramic membrane treatment: the filtering aperture of the ceramic membrane can be selected to be 20-500 nm. The filtration pressure of the membrane equipment is 0.5Mpa, the temperature is 50 ℃, and the flow velocity of the membrane surface is 4 m/s. Sending the pretreated crude peanut oil into first-stage ceramic membrane equipment through a feeding pump, filtering by a ceramic membrane, intercepting impurities such as colloid and suspended matters, and collecting clean peanut oil into a ceramic membrane clear liquid tank by penetrating through the first-stage ceramic membrane under the drive of pressure. And feeding the first-stage ceramic membrane concentrated solution serving as a raw material into second-stage ceramic membrane equipment, and collecting the clean peanut oil to a ceramic membrane clear solution tank through a second-stage ceramic membrane under the drive of pressure. And feeding the second-stage ceramic membrane concentrated solution serving as a raw material into a third-stage ceramic membrane device, and collecting the clean peanut oil to a ceramic membrane clear solution tank through a third-stage ceramic membrane under the driving of pressure. And by parity of reasoning, the ceramic membrane concentrated solution of the last stage enters a ceramic membrane concentrated solution tank.
(3) Treating a ceramic membrane concentrated solution: and (4) feeding the ceramic membrane concentrated solution into a centrifugal machine for separation, and removing impurities such as colloid, suspended matters and the like. The centrifugation time is 20min and the rotation speed is 8000 rpm. Returning the obtained clear liquid of the centrifuge to the ceramic membrane raw material tank, continuously filtering, and returning the thick slag of the centrifuge to the squeezing working section.
(4) Clean peanut oil collected in the clear liquid tank: the physicochemical indexes (color, moisture and volatile matter, acid value, peroxide value and heating experiment (280 ℃)) meet the first-grade standard (GB/T1534-; the retention rate of VE and sterol functional components reaches over 96 percent, and the retention rate of total unsaturated fatty acid reaches 95 percent; in terms of flavor, the special flavor of the peanut oil is reserved, and the flavor substances mainly comprise nitrogen-containing and oxygen-containing heterocyclic compounds such as pyrazine, pyridine, furan, pyrrole and the like, and aldehydes, ketones, alcohols, acids, esters and hydrocarbon compounds. The number of types of these flavors is the same as that of peanut crude oil, and the retention rate of each type of compound is as high as 99%.
Example 3: preparation method of grease with high retention of functional components and flavor
A method for preparing grease with high retention of functional components and flavor,
the filter element of the ceramic membrane filter is a modified tubular multi-channel ceramic membrane;
the method for modifying the modified tubular multi-channel ceramic membrane comprises the following steps: soaking the tubular multi-channel ceramic membrane in pure water for 12 hours, drying the tubular multi-channel ceramic membrane in an oven for 10 hours, and filling the tubular multi-channel ceramic membrane into a ceramic membrane component to form a ceramic membrane filter; dissolving an organosilane coupling agent in absolute ethyl alcohol, and stirring for 30 minutes to obtain an ethanol solution of the organosilane coupling agent;
preheating the tubular multi-channel ceramic membrane to 85 ℃, heating and gasifying an ethanol solution of the organosilane coupling agent, and then contacting the coupling agent with the tubular multi-channel ceramic membrane to modify the tubular multi-channel ceramic membrane to obtain a modified tubular multi-channel ceramic membrane;
the preparation method comprises the following steps:
step 1: pretreating the crude oil to obtain pretreated crude oil; the pretreatment adopts one of the following two oil pretreatment methods:
the pretreatment method comprises the following steps: filtering the crude oil, heating to 60 ℃, adding hot water at 60 ℃ accounting for 0.3 percent of the weight of the crude oil, uniformly stirring, and standing and settling for 3 hours at 60 ℃ to complete hydration;
and a second pretreatment method: preheating crude oil at 60 ℃, adding 15mL of citric acid buffer solution into each kilogram of crude oil, homogenizing, and stirring for 10 min; cooling to 40 ℃, adding an enzymatic reaction catalyst with the mass of 0.4% of that of the crude oil, homogenizing, and carrying out degumming reaction for 2 hours in a water bath kettle at 40 ℃ under the stirring condition; after the reaction is finished, the immobilized enzyme is recovered because the immobilized enzyme is adopted in the embodiment; the enzymatic reaction catalyst is prepared by mixing distilled water, protease and phospholipase according to the ratio of 10: 1: 5 in mass ratio;
step 2: connecting 5 ceramic membrane filters in series, and then filtering the pretreated crude oil, wherein the filtering pressure is 0.05Mpa, the temperature is 20 ℃, and the membrane surface flow rate is 1 m/s/s; the pretreated crude oil is pumped into a first-stage ceramic membrane filter, clean oil permeates the first-stage ceramic membrane filter under the pressure drive and is collected into a ceramic membrane clear liquid tank, concentrated solution obtained by the first-stage ceramic membrane filter is sent into a second-stage ceramic membrane filter as raw material, the clean oil permeates a second-stage ceramic membrane under the pressure drive and is collected into the ceramic membrane clear liquid tank, concentrated solution obtained by the second-stage ceramic membrane filter is sent into a third-stage ceramic membrane filter as raw material, the clean oil permeates the third-stage ceramic membrane filter under the pressure drive and is collected into the ceramic membrane clear liquid tank, and the rest is done by analogy, and concentrated solution obtained by the last-stage ceramic membrane filter enters the ceramic membrane concentrated liquid tank;
and step 3: feeding the concentrated solution obtained by the last stage of ceramic membrane filter stored in the ceramic membrane concentrated solution tank into a centrifuge for centrifugal separation; returning the obtained clear liquid to the ceramic membrane raw material tank, and continuously filtering; returning the thick slag of the centrifuge to the squeezing section.
The preferred embodiment is: the tubular multi-channel ceramic membrane is formed by sintering zirconia, titania and silica at high temperature; the aperture of the tubular multi-channel ceramic membrane is 0.02 micron.
The preferred embodiment is: the homogenizing treatment rate is 10000r/min, and the treatment time is 0.5-1.5 min.
The preferable technical scheme is as follows: the protease is immobilized protease; the phospholipase is immobilized phospholipase.
The preferred embodiment is: also included is a modified tubular multichannel ceramic membrane apparatus: the outlet of the ceramic membrane filter is communicated with an air inlet pipe of a vacuum pumping system through a first pipeline; the inlet of the ceramic membrane filter is communicated with the air outlet of an air heating system through a second pipeline, and the path of the second pipeline is communicated with a storage tank for storing an ethanol solution of an organosilane coupling agent through a third pipeline, as shown in fig. 1.
The preferred embodiment is: the crude oil is hot-pressed peanut oil, corn germ oil and cottonseed oil, and the weight ratio of the crude oil to the raw oil is 1: 1: 1, and the phospholipid content is 350 mg/kg.
The preferred embodiment is: before the ceramic membrane filter is used, firstly, baking the modified tubular multichannel ceramic membrane in a 70 ℃ oven for 1h, then, carrying out oil rinsing on the tubular multichannel ceramic membrane by adopting refined first-grade grease at the pressure difference of 0.1Mpa MPa, the temperature of 20 ℃ and the flow rate of 1m/s/s so as to stabilize the performance of the tubular multichannel ceramic membrane; the grease is rapeseed oil.
The preferable technical scheme is as follows: filtering the pretreated crude oil by using a vertical leaf filter or a metal pipe network filter; the filtration precision is 10 meshes, and the filtration pressure is 0.05 Mpa.
The preferable technical scheme is as follows: the cleaning solution adopted by the tubular multi-channel ceramic membrane is refined first-grade grease; the grease is rice bran oil; the cleaning method comprises the following steps: adding 8 liters of cleaning solution into the ceramic membrane filter, starting the ceramic membrane filter, and carrying out reflux operation for 30min under the conditions that: the membrane pressure difference is 0.1Mpa, the temperature is 25 ℃, and the flow rate is 1 m/; the operation was repeated twice.
Different fats and oils have different characteristic flavors for their characteristic flavors. The oil material can present a plurality of different flavor substances in the thick fragrant oil obtained by pressing after frying. The source of the flavor substances mainly comprises 3 types of sources, namely (1) Maillard reaction between amino acid and sugar, (2) oxidation reaction of fat and (3) sugar degradation reaction. Wherein, Maillard reaction is an important way for generating flavor substances in the food processing process, and products thereof mainly comprise nitrogen-oxygen heterocyclic compounds, such as pyrazine pyrrole pyridine compounds and the like; the oxidation reaction of fat is an inevitable reaction for generating flavor in the hot pressing process of oil materials, and main products of the oxidation reaction are acid, aldehyde, ketone, hydrocarbon compounds and the like; the sugar degradation reaction can form carbonyl, olefin, acid, furan and pyran compounds. The treatment method of this example retained a large amount of these functional components and flavors.
Example 4: preparation method of grease with high retention of functional components and flavor
A method for preparing grease with high retention of functional components and flavor,
the filter element of the ceramic membrane filter is a modified tubular multi-channel ceramic membrane;
the method for modifying the modified tubular multi-channel ceramic membrane comprises the following steps: soaking the tubular multi-channel ceramic membrane in pure water for 24 hours, drying the tubular multi-channel ceramic membrane in an oven for 6 hours, and filling the tubular multi-channel ceramic membrane into a ceramic membrane component to form a ceramic membrane filter; dissolving an organosilane coupling agent in absolute ethyl alcohol, and stirring for 60 minutes to obtain an ethanol solution of the organosilane coupling agent;
preheating the tubular multi-channel ceramic membrane to 90 ℃, heating and gasifying an ethanol solution of the organosilane coupling agent, and then contacting the coupling agent with the tubular multi-channel ceramic membrane to modify the tubular multi-channel ceramic membrane to obtain a modified tubular multi-channel ceramic membrane;
the preparation method comprises the following steps:
step 1: pretreating the crude oil to obtain pretreated crude oil; the pretreatment adopts one of the following two oil pretreatment methods:
the pretreatment method comprises the following steps: filtering the crude oil, heating to 80 ℃, adding 80 ℃ hot water accounting for 0.5 percent of the weight of the crude oil, uniformly stirring, and standing and settling for 5 hours at 80 ℃ to complete hydration;
and a second pretreatment method: preheating crude oil at 80 ℃, adding 25mL of citric acid buffer solution into each kilogram of crude oil, homogenizing, and stirring for 20 min; cooling to 55 ℃, adding an enzymatic reaction catalyst with the mass of 0.6 percent of that of the crude oil, homogenizing, and carrying out degumming reaction for 4 hours in a water bath kettle at 55 ℃ under the stirring condition; after the completion of the reaction, the enzyme was inactivated by heating since the enzyme reaction catalyst of this example contained free phospholipase;
step 2: connecting 10 ceramic membrane filters in series, and then filtering the pretreated crude oil, wherein the filtering pressure is 1Mpa, the temperature is 80 ℃, and the membrane surface flow rate is 6 m/s; the pretreated crude oil is pumped into a first-stage ceramic membrane filter, clean oil permeates the first-stage ceramic membrane filter under the pressure drive and is collected into a ceramic membrane clear liquid tank, concentrated solution obtained by the first-stage ceramic membrane filter is sent into a second-stage ceramic membrane filter as raw material, the clean oil permeates a second-stage ceramic membrane under the pressure drive and is collected into the ceramic membrane clear liquid tank, concentrated solution obtained by the second-stage ceramic membrane filter is sent into a third-stage ceramic membrane filter as raw material, the clean oil permeates the third-stage ceramic membrane filter under the pressure drive and is collected into the ceramic membrane clear liquid tank, and the rest is done by analogy, and concentrated solution obtained by the last-stage ceramic membrane filter enters the ceramic membrane concentrated liquid tank;
and step 3: feeding the concentrated solution obtained by the last stage of ceramic membrane filter stored in the ceramic membrane concentrated solution tank into a centrifuge for centrifugal separation; returning the obtained clear liquid to the ceramic membrane raw material tank, and continuously filtering; returning the thick slag of the centrifuge to the squeezing section.
The preferred embodiment is: the tubular multi-channel ceramic membrane is formed by sintering zirconia at high temperature; the aperture of the tubular multi-channel ceramic membrane is 0.5 micron.
The preferred embodiment is: the homogenizing treatment rate is 20000r/min, and the treatment time is 1.5 min.
The preferred embodiment is: the protease is free protease or immobilized protease.
The preferred embodiment is: also included is a modified tubular multichannel ceramic membrane apparatus: the outlet of the ceramic membrane filter 1 is communicated with an air inlet pipe of a vacuum pumping system 2 through a first pipeline; the inlet of the ceramic membrane filter is communicated with the air outlet of an air heating system 3 through a second pipeline, the path of the second pipeline is communicated with a storage tank 4 for storing ethanol solution of organosilane coupling agent through a third pipeline, as shown in figure 1, the hydrophobic modified tubular multi-channel ceramic membrane is prepared by chemical grafting modification by adopting organosilane coupling agent, and the modification method is a gas phase method. Soaking the ceramic membrane in pure water for 12-24 hours, drying in an oven at 120 ℃ for more than 6 hours, and filling into the ceramic membrane component for later use. Dissolving the organosilane coupling agent in absolute ethyl alcohol, and stirring and reacting for 30-60 minutes for later use. The heating system is connected with the membrane component, and the outlet of the membrane component is connected with the vacuum system. The whole system is preheated to more than 80 ℃, the ethanol solution is gradually injected into a heating system for gasification, the coupling agent is contacted and reacted with the ceramic membrane through a vacuum system, unreacted ethanol and the coupling agent are discharged through the vacuum system, and the modified ceramic membrane can be directly used after being simply dried for 1 hour at 120 ℃. Examples of organosilane coupling agents are: octadecyl trichlorosilane, hexadecyltrichlorosilane, octyl trichlorosilane and a silane coupling agent KH 570.
The preferred embodiment is: the crude oil is hot-pressed maize germ oil, and the phospholipid content of the crude oil is 400 mg/kg.
The preferred embodiment is: before the ceramic membrane filter is used, firstly, baking the modified tubular multichannel ceramic membrane in a 70 ℃ oven for 1h, then, adopting refined four-grade grease, and carrying out oil rinsing on the tubular multichannel ceramic membrane at the pressure difference of 0.8Mpa, the temperature of 80 ℃ and the flow rate of 6m/s to ensure that the performance of the tubular multichannel ceramic membrane is stable; the oil is rice bran oil.
The preferred embodiment is: filtering the pretreated crude oil by using a vertical leaf filter or a metal pipe network filter; the filtration precision is 500 meshes, and the filtration pressure is 1 Mpa.
The preferred embodiment is: the cleaning solution adopted by the tubular multi-channel ceramic membrane is refined four-stage grease; the oil rice bran oil; the cleaning method comprises the following steps: adding 12 liters of cleaning solution into the ceramic membrane filter, starting the ceramic membrane filter, and carrying out reflux operation for 60min under the conditions that: the membrane pressure difference is 0.3Mpa, the temperature is 60 ℃, and the flow rate is 6 m/s; the operation was repeated three times.
The foregoing is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting thereof in any way, and any modifications or variations thereof that fall within the spirit of the invention are intended to be included within the scope thereof.
Claims (9)
1. A method for preparing grease with high retention of functional components and flavor is characterized in that:
the filter element of the ceramic membrane filter is a modified tubular multi-channel ceramic membrane;
the method for modifying the modified tubular multi-channel ceramic membrane comprises the following steps: soaking the tubular multi-channel ceramic membrane in pure water for 12-24 hours, drying the tubular multi-channel ceramic membrane in an oven for more than 6 hours, and filling the tubular multi-channel ceramic membrane into a ceramic membrane component to form a ceramic membrane filter; dissolving an organosilane coupling agent in absolute ethyl alcohol, and stirring for 30-60 minutes to obtain an ethanol solution of the organosilane coupling agent;
preheating the tubular multi-channel ceramic membrane to above 80 ℃, heating and gasifying an ethanol solution of the organosilane coupling agent, and then contacting the coupling agent with the tubular multi-channel ceramic membrane to modify the tubular multi-channel ceramic membrane to obtain a modified tubular multi-channel ceramic membrane;
the preparation method comprises the following steps:
step 1: pretreating the crude oil to obtain pretreated crude oil; the pretreatment adopts one of the following two oil pretreatment methods:
the pretreatment method comprises the following steps: filtering the crude oil, heating to 60-80 deg.C, adding 60-80 deg.C hot water 0.3-0.5% of crude oil weight, stirring, standing at 60-80 deg.C for 3-5 hr to complete hydration;
and a second pretreatment method: preheating crude oil at 60-80 deg.C, adding citric acid buffer solution 15-25mL per kg crude oil, homogenizing, and stirring for 10-20 min; cooling to 40-55 deg.C, adding enzymatic reaction catalyst 0.4-0.6% of crude oil, homogenizing, and degumming in 40-55 deg.C water bath under stirring for 2-4 hr; after the reaction is finished, if the enzymatic reaction catalyst contains free phospholipase, heating to inactivate the enzyme, and if immobilized enzyme is adopted, recovering the immobilized enzyme; the enzymatic reaction catalyst is formed by mixing distilled water with at least one of protease and phospholipase;
step 2: connecting a plurality of ceramic membrane filters in series, and then filtering the pretreated crude oil, wherein the filtering pressure is 0.05-1 Mpa, the temperature is 20-80 ℃, and the membrane surface flow rate is 1-6 m/s; the pretreated crude oil is pumped into a first-stage ceramic membrane filter, clean oil permeates the first-stage ceramic membrane filter under the pressure drive and is collected into a ceramic membrane clear liquid tank, concentrated solution obtained by the first-stage ceramic membrane filter is sent into a second-stage ceramic membrane filter as raw material, the clean oil permeates a second-stage ceramic membrane under the pressure drive and is collected into the ceramic membrane clear liquid tank, concentrated solution obtained by the second-stage ceramic membrane filter is sent into a third-stage ceramic membrane filter as raw material, the clean oil permeates the third-stage ceramic membrane filter under the pressure drive and is collected into the ceramic membrane clear liquid tank, and the rest is done by analogy, and concentrated solution obtained by the last-stage ceramic membrane filter enters the ceramic membrane concentrated liquid tank;
and step 3: feeding the concentrated solution obtained by the last stage of ceramic membrane filter stored in the ceramic membrane concentrated solution tank into a centrifuge for centrifugal separation; returning the obtained clear liquid to the ceramic membrane raw material tank, and continuously filtering; returning the thick slag of the centrifuge to the squeezing section.
2. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: the tubular multi-channel ceramic membrane is formed by sintering at least one material of alumina, zirconia, titania and silica at high temperature; the aperture of the tubular multi-channel ceramic membrane is 0.02-0.5 microns.
3. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: the homogenizing treatment rate is 10000-20000 r/min, and the treatment time is 0.5-1.5 min.
4. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: the protease is free protease or immobilized protease; the phospholipase is free phospholipase or immobilized phospholipase.
5. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: the device also comprises a device for modifying the tubular multi-channel ceramic membrane: the outlet of the ceramic membrane filter is communicated with an air inlet pipe of a vacuum pumping system through a first pipeline; the inlet of the ceramic membrane filter is communicated with the air outlet of an air heating system through a second pipeline, and the path of the second pipeline is communicated with a storage tank for storing ethanol solution of the organosilane coupling agent through a third pipeline.
6. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: the crude oil is at least one of hot pressed rapeseed oil, soybean oil, peanut oil, corn germ oil, cottonseed oil, rice bran oil, sunflower seed oil, tea seed oil and other vegetable oil crude oil, and the phospholipid content is 80-400 mg/kg.
7. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: before the ceramic membrane filter is used, firstly, baking the modified tubular multichannel ceramic membrane in a baking oven at 70 ℃ for 1h, then, carrying out oil rinsing on the tubular multichannel ceramic membrane by adopting refined first-level, second-level, third-level and fourth-level grease at the pressure difference of 0.1-0.8 Mpa, the temperature of 20-80 ℃ and the flow rate of 1-6 m/s so as to stabilize the performance of the tubular multichannel ceramic membrane; the oil is rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, rice bran oil, sunflower seed oil or tea seed oil.
8. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: filtering the pretreated crude oil by using a vertical leaf filter or a metal pipe network filter; the filtration precision is 10-500 meshes, and the filtration pressure is 0.05-1 Mpa.
9. The method for producing a functional ingredient-and flavor-retaining fat or oil according to claim 1, wherein the method comprises the steps of: cleaning solution adopted by the tubular multi-channel ceramic membrane is refined first-level, second-level, third-level and fourth-level grease; the oil is rapeseed oil, soybean oil, peanut oil, corn oil, cottonseed oil, rice bran oil, sunflower seed oil or tea seed oil; the cleaning method comprises the following steps: adding 8-12 liters of cleaning solution into the ceramic membrane filter, starting the ceramic membrane filter, and carrying out reflux operation for 30-60min under the conditions that: the membrane pressure difference is 0.1-0.3 Mpa, the temperature is 25-60 ℃, and the flow rate is 1-6 m/s; the operation is repeated at least once.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590927A (en) * | 2017-01-08 | 2017-04-26 | 山东乐悠悠花生油科技有限公司 | Fine finishing method for high-quality peanut oil |
| CN106669440A (en) * | 2017-01-03 | 2017-05-17 | 中国石油天然气股份有限公司 | Modification method of ceramic membrane and modified ceramic membrane |
| WO2018112599A1 (en) * | 2016-12-23 | 2018-06-28 | Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources | Modified ceramic membranes for treatment of oil sands produced water, discharge water and effluent streams |
| CN108699488A (en) * | 2015-12-17 | 2018-10-23 | 佛兰芒技术研究所有限公司 | Detach unsaturated organic compound |
| CN109694776A (en) * | 2018-12-28 | 2019-04-30 | 合肥工业大学 | The method of vegetable oil degumming |
-
2019
- 2019-11-22 CN CN201911152408.XA patent/CN110835582A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108699488A (en) * | 2015-12-17 | 2018-10-23 | 佛兰芒技术研究所有限公司 | Detach unsaturated organic compound |
| WO2018112599A1 (en) * | 2016-12-23 | 2018-06-28 | Her Majesty The Queen In Right Of Canada As Represented By The Minister Of Natural Resources | Modified ceramic membranes for treatment of oil sands produced water, discharge water and effluent streams |
| CN106669440A (en) * | 2017-01-03 | 2017-05-17 | 中国石油天然气股份有限公司 | Modification method of ceramic membrane and modified ceramic membrane |
| CN106590927A (en) * | 2017-01-08 | 2017-04-26 | 山东乐悠悠花生油科技有限公司 | Fine finishing method for high-quality peanut oil |
| CN109694776A (en) * | 2018-12-28 | 2019-04-30 | 合肥工业大学 | The method of vegetable oil degumming |
Non-Patent Citations (1)
| Title |
|---|
| 高能文 等: "陶瓷膜表面疏水改性对过滤性能的影响", 《第四届中国膜科学与技术报告会论文集第四届中国膜科学与技术报告会论文集》, 31 October 2010 (2010-10-31), pages 440 - 443 * |
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