CN107011991B - A kind of cation resin dephosphorization method of grease - Google Patents
A kind of cation resin dephosphorization method of grease Download PDFInfo
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- CN107011991B CN107011991B CN201710236937.2A CN201710236937A CN107011991B CN 107011991 B CN107011991 B CN 107011991B CN 201710236937 A CN201710236937 A CN 201710236937A CN 107011991 B CN107011991 B CN 107011991B
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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
- C11B3/02—Refining fats or fatty oils by chemical reaction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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Abstract
本发明公开的一种油脂的阳离子树脂脱磷方法，将待处理的油脂先与强酸性阳离子树脂充分接触，再将处理后的油脂通过水化脱磷法去除磷脂，得到脱磷后的油脂。该方法仅采用强酸性阳离子树脂对油脂进行处理，磺酸型阳离子交换树脂具有固体强酸的特性，可将磷脂酸的金属盐转化为磷脂酸，再经后续的水化脱磷而除去。通过这种方式，既可除去油脂中的水化磷脂，又可除去油脂中的非水化磷脂，从而显著提高了油脂的脱磷效果，有效地保证了脱磷油的质量。本发明工艺流程短、操作简单、经济、环保、脱磷效率高。
The invention discloses a cation resin dephosphorization method for oil and fat. The oil to be treated is fully contacted with a strong acid cation resin, and then the treated oil is removed by a hydration dephosphorization method to remove phospholipids to obtain dephosphorized oil. The method only uses a strong acid cation resin to treat the oil, and the sulfonic acid type cation exchange resin has the characteristics of solid strong acid, which can convert the metal salt of phosphatidic acid into phosphatidic acid, and then remove it by subsequent hydration and dephosphorization. In this way, both the hydrated phospholipid in the oil and the non-hydratable phospholipid in the oil can be removed, thereby significantly improving the dephosphorization effect of the oil and effectively ensuring the quality of the dephosphorized oil. The invention has short technological process, simple operation, economy, environmental protection and high dephosphorization efficiency.
Description
Technical Field
The invention belongs to the technical field of oil refining, relates to a method for dephosphorizing grease by using cationic resin, and particularly relates to a method for dephosphorizing grease by using strong-acid cationic resin.
Background
Phospholipid is a common impurity in crude oil and can form peptization impurities with protein, mucus, trace metals and the like in oil. These colloidal impurities have poor high temperature stability, are easily oxidized to become black, scorched and bitter, and are fuming and bubbling in the cooking process. And the oxidative discoloration of the grease can be accelerated in the storage process, and the shelf life of the grease is shortened. Therefore, the phospholipids must be removed during the refining process of the oil and fat, which is called dephosphorization of crude oil.
In addition, the grease is used as a direct raw material of the biodiesel, and phosphorus in the grease can directly influence the phosphorus content of the biodiesel. In view of the fact that phosphorus in biodiesel poisons a diesel engine exhaust catalyst and increases the emission of pollutants, the phosphorus content of biodiesel is clearly limited in various main countries and regions of the world including China, and the phosphorus content of biodiesel is not higher than 10mg/kg (namely 10ppm) as specified in GB/T20828 2015 (biodiesel for diesel fuel blending (BD 100)). This also puts requirements on the phosphorus content of the grease, the raw material of biodiesel.
Phospholipids can be classified into two groups according to their affinity for water, namely, Hydrated Phospholipids (HP) and non-hydrated phospholipids (NHP). The hydrated phospholipid has the characteristics of water absorption expansion and aggregation into colloidal particles, and can be removed by firstly stirring with water and then centrifuging or standing for sedimentation. The non-hydrated phospholipid is mainly metal salt of phosphatidic acid, exists in the forms of calcium phosphatidate, magnesium phosphatidate, ferric phosphatidate, copper phosphatidate and the like, and has obvious hydrophobicity, so that the hydrated dephosphorization method is not effective. Heavy metals in non-hydrated phospholipids are detrimental to human health. The copper phosphatidate, the iron phosphatidate and the like can catalyze the oxidation reaction of the grease, and accelerate the rancidity and the odor of the grease. Therefore, how to economically and effectively remove the non-hydrated phospholipid is always a difficult point and a hot point for dephosphorizing the grease.
Frank D. Gunstone et al in The Lipid Handbook (3)rdEdtion, CRC Press, London, p180), gives the charge status of phospholipids at different pH as shown in the following table:
+: the molecule has a positive charge
(+): most of the molecules have a positive charge
(±): most of the molecules being zwitterions
+ -: the molecule being a zwitterion
0: no charge on the molecule
(-): most of the molecules have a negative charge
-: the molecule has a negative charge
2-: the molecule has two negative charges
Zhaowanli et al (dynamic and thermodynamic studies on degumming behavior of weak acid type ion exchange resins, Chinese fats 2012,37(9):27-30) performed direct dephosphorization of pepper seed oil using weak acid cation exchange resins. Research shows that weak acid ion exchange resin can directly remove phospholipid, but has the following defects:
1) the process is not effective on non-hydrated phospholipids, which is just the difficulty of grease dephosphorization. As for non-hydrated phospholipid (the principle is shown in figure 2), since the functional group of the weak acidic resin is carboxylic acid, the acidity is weaker than that of the phosphate group on the right phosphatidic acid in the reaction formula, and the reaction is difficult to carry out according to the basic chemical common knowledge that the weak acid can not prepare strong acid. For the hydrated phospholipids (see the principle in figure 1). The reaction is possible, but because it is based on ion exchange, only phospholipids in cationic form with positive charge in the oil can be removed. As can be seen from Table 1, only two types of hydrated phospholipids, phosphatidylcholine (PC for short) and phosphatidylethanolamine (PE for short), are likely to be in the form of cations. Therefore, the weak acid cation exchange resin can be effective to the easily removed hydrated phospholipid PC or PE only under certain conditions, but is ineffective to the non-hydrated phospholipid;
2) the method has poor dephosphorization effect. The final phospholipid content is still as high as 2.0849g/kg (namely 2085ppm, and the conversion is about 80ppm in terms of phosphorus content), and the requirement is difficult to meet;
3) the cost is too high. The ratio of the resin usage amount to the grease for the best dephosphorization effect is 0.38:1 (weight ratio), that is, 1kg of weak acidic resin can only treat 2.63kg of crude oil, and the treatment amount is too low, which inevitably leads to poor economy of the method and difficult industrial application.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the grease cationic resin dephosphorization method which is short in process flow, simple to operate, green and environment-friendly and remarkable in dephosphorization effect.
The invention is realized by the following technical scheme:
the invention discloses a grease dephosphorization method by using cationic resin, which comprises the steps of fully contacting grease to be treated with strong acid cationic resin, and removing phospholipid from the treated grease by using a hydration dephosphorization method to obtain dephosphorized grease;
wherein the functional group of the strong acid cation resin is-SO3H。
Preferably, the sufficient contact is to mix the oil to be treated directly with the strongly acidic cation resin or to flow the oil to be treated through a column packed with the strongly acidic cation resin.
Preferably, the grease and the strong acid cation resin are directly mixed, and the specific operations are as follows:
adding strong acid cation resin with the mass of 1-10% of that of the grease into the grease to be treated, and shaking for 5-8 h in a shaking table at constant temperature under the conditions of 60 ℃ and 200 r/min.
Preferably, the grease to be treated is passed through a column packed with a strongly acidic cation resin by: the method is characterized in that grease to be treated continuously flows through a column filled with strong acid cation resin at the flow rate of 1BV/h, and effluent liquid is collected at an outlet of the column.
Further preferably, the collecting operation is ended when calcium ions leak out of the effluent and are less than 5 ppm.
Further preferably, the strongly acidic cation resin is capable of being regenerated, the regeneration method comprising the steps of:
1) using distilled water with the volume of 2BV to pass through the column to replace grease in the column, wherein the flow rate is 1BV/h, and the flow direction is from bottom to top;
2) using 2-2.5 BV H10% by volume2SO4Enabling the solution to flow through the column at the flow rate of 2BV/h and in the flow direction from bottom to top;
3) passing distilled water with the volume of 2BV through the column at the flow rate of 2BV/h in the flow direction from top to bottom;
4) 2BV of refined oil is used for passing through the column, the water in the column is replaced, the flow rate is 2BV/h, and the flow direction is from top to bottom.
Preferably, the hydration dephosphorization method is to add softened hot water which accounts for 5 percent of the volume of the grease, 80 ℃ and pH value of 5-8 into the grease treated by the strong acid cation resin, shake the grease in a shaking table at constant temperature of 80-85 ℃ and 200r/min for 20-45 min, and then centrifuge the grease for 20min at 8000 r/min.
Preferably, the grease to be treated is subjected to hydration dephosphorization treatment before being fully contacted with the strong acid cation resin.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention discloses a grease dephosphorization method by using cationic resin, which comprises the steps of fully contacting grease to be treated with strong acid cationic resin, and removing phospholipid from the treated grease by using a hydration dephosphorization method to obtain the grease after dephosphorization. The grease is treated by strong acid cation resin, and the sulfonic acid type cation exchange resin has the characteristic of solid strong acid, can convert metal salt of phosphatidic acid into phosphatidic acid, and is removed by subsequent hydration dephosphorization. By the method, not only can hydrated phospholipid in the grease be removed, but also non-hydrated phospholipid in the grease can be removed, so that the dephosphorization effect of the grease is obviously improved, and the quality of the dephosphorized oil is effectively ensured. The method has the advantages of short process flow, simple operation, economy, environmental protection and high dephosphorization efficiency.
Furthermore, before the grease to be treated is fully contacted with the strong acid cation resin, the grease to be treated is firstly subjected to hydration dephosphorization treatment, and a three-stage grease dephosphorization process of hydration dephosphorization, strong acid cation resin conversion and hydration dephosphorization is adopted, so that PC and other positively charged hydrated phospholipids in the grease are removed in the first step of hydration dephosphorization, and the strong acid cation resin in the second step mainly plays a role in converting non-hydrated phospholipids into phosphatidic acid instead of directly removing the hydrated phospholipids, thereby lightening the burden of the resin, remarkably reducing the using amount of the resin, effectively prolonging the service life of the resin and further reducing the cost.
Drawings
FIG. 1 is a schematic diagram showing the reaction for removing hydrated phospholipids of Zhao Wanli et al;
FIG. 2 is a schematic diagram showing the removal reaction of non-hydrated phospholipids of Zhao Wanli et al;
FIG. 3 is a schematic diagram of the removal reaction of hydrated phospholipids to remove non-hydrated phospholipids in accordance with the present invention;
FIG. 4 is a schematic diagram of the removal reaction of non-hydrated phospholipids in accordance with the present invention.
Detailed Description
The following examples are intended to further illustrate the invention but are not intended to represent the only way to practice the invention and are not intended to be limiting.
Referring to fig. 2, the general idea of the present invention is: the sulfonic acid type strong acid cation resin can perform double decomposition reaction with salt to remove metal of metal phosphate (the principle is shown in figure 4), non-hydrated phospholipid which is difficult to remove is converted into hydrated phospholipid, and the hydrated phospholipid is removed by hydration dephosphorization with low cost. The resin here acts as a conversion rather than a direct removal of the hydrated phospholipids.
The reaction of FIG. 3 of the present invention can also occur, i.e., the strongly acidic cationic resin also has a direct removal effect on the hydrated phospholipids. However, since the electrostatic force between the cationic resin and the divalent ion is stronger than that of monovalent hydrated phospholipid, in other words, the affinity of the resin to the divalent metal ion is stronger than that of monovalent hydrated phospholipid, the main reaction is shown in FIG. 4.
In order to further improve the utilization rate of the resin, i.e. reduce the reaction in fig. 3, the reaction in fig. 4 is fully utilized, firstly hydrated phospholipid with positive charge is removed by hydration dephosphorization, then non-hydrated phospholipid is converted into phosphatidic acid by the conversion of the resin, and finally the hydrated phospholipid is removed by hydration dephosphorization.
After the grease is treated by the strong acid cation resin, the pH value of softened hot water in the hydration dephosphorization is controlled within the range of 5-8 in the subsequent hydration dephosphorization process, so that phosphatidic acid can be more easily dissociated and is negatively charged for removal. Thereby achieving better dephosphorization effect.
Example 1
Application of sulfonic acid type cationic resin Amberlite 200C + hydration dephosphorization in rapeseed crude oil dephosphorization experiment
The method used in this example:
20mL of rapeseed crude oil (phosphorus content: 384.2ppm) was put in a shake flask, and 2g of-SO as a functional group was added3H Amberlite 200C resin (Rohm and Haas, USA). The shake flask was placed in a shaker and shaken at 60 ℃ at a constant temperature of 200r/min for 6 h. Then taking out the oil phase, adding softened hot water with the pH value of 5.0 at 80 ℃ and 5% vol into the oil phase, and shaking at the constant temperature of 80 ℃ and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain refined oil.
The final phosphorus content after the treatment by the method is 26.8ppm, and the specific parameters are shown in Table 1.
Hydration dephosphorization: for comparison, the rapeseed crude oil was directly dephosphorized by hydration. The concrete conditions are as follows: 20mL of rapeseed crude oil was put in a shake flask, and softened hot water at 80 ℃ and 5% vol was added thereto. Shaking at 80 deg.C and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain refined oil. The final phosphorus content was 124.6ppm, see in particular Table 2.
TABLE 1 treatment of crude rapeseed oil by the Process of the invention (Amberlite 200C resin-dephosphorization by hydration)
TABLE 2 treatment of crude rapeseed oil by a hydration dephosphorization process
Obviously, the method adopted by the invention has obvious advantages, and compared with the traditional hydration dephosphorization process, the method has obvious dephosphorization effect; compared with the method of Zhao Wanli et al, the invention greatly reduces the resin dosage and has better dephosphorization effect.
Example 2
Sulfonic acid type cationic resin Amberlite FPC22+ hydration dephosphorization experiment for soybean crude oil dephosphorization
20mL of crude soybean oil (phosphorus content: 126.7ppm) was put in a shake flask, and 1g of-SO as a functional group was added3H Amberlite FPC22 resin (Rohm and Haas company, USA), the flask was placed in a shaker and shaken at 60 ℃ at 200r/min for 6H. Then taking out the oil phase, adding 5 percent of the oil phasevol, softened hot water with pH of 6.0 at 80 deg.C, and shaking at constant temperature of 80 deg.C and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain refined oil.
The final phosphorus content after the treatment by the method is 2.7ppm, and the specific parameters are shown in Table 3.
Hydration dephosphorization: for comparison, crude soybean oil was directly dephosphorized by hydration. The concrete conditions are as follows: 20mL of crude soybean oil was put in a shake flask, and softened hot water at 80 ℃ and 5% vol was added thereto. Shaking at 80 deg.C and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain refined oil. The final phosphorus content was 43.0ppm, see in particular Table 4.
TABLE 3 treatment of crude Soybean oil by the Process of the invention (Amberlite FPC22 resin-Hydrophosphorization)
TABLE 4 treatment of crude soybean oil by hydration dephosphorization process
Example 3
Sulfonic acid type cationic resin Amberlite 252+ hydration dephosphorization experiment for dephosphorizing pepper seed crude oil
20mL of Amberlite 252 resin (Rohm and Haas company, USA) is taken and filled into a column (the diameter of the column is 1cm, the length of the column is 25cm), crude pepper seed oil (phosphorus content: 233.5ppm) is continuously pumped into the column at the flow rate of 0.3mL/min, collection is stopped when the calcium ion leakage concentration at the outlet of the column reaches 2ppm, and 3000mL of pepper seed oil is collected totally. Taking 100mL of resin-treated pricklyash seed oil, adding 5% vol softened hot water with pH of 7.0 at 80 ℃, and shaking at constant temperature of 80 ℃ and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain refined oil.
The final phosphorus content after treatment by this method was 0.5 ppm.
Regenerating the used resin, wherein the specific process comprises the following steps:
(1) using 40mL of distilled water to pass through the column to replace grease in the column, wherein the flow rate is 0.3mL/min, and the flow direction is from bottom to top;
(2) 40mL of 10% H were used2SO4Enabling the solution to flow through the column at the flow rate of 0.6mL/min and in the flow direction from bottom to top;
(3) 40mL of distilled water is used for passing through the column, the flow rate is 0.6mL/min, and the flow direction is from top to bottom;
(4) 40mL of refined prickly ash seed oil is used for passing through the column to replace the water in the column, the flow rate is 0.6mL/min, and the flow direction is from top to bottom. And finishing resin regeneration for later use.
Dephosphorizing by using weak acid resin: in order to compare the method of using weak acid cation exchange resin by Zhaowanli et al, 20mL of Amberlite 3500 resin (Rohm and Haas company, USA) is taken and filled into a column (the column diameter is 1cm, the column length is 25cm), crude pricklyash seed oil (phosphorus content: 233.5ppm) is continuously pumped into the column, the flow rate is 0.3mL/min, when the phosphorus content of oil at the outlet of the column is equivalent to that of oil at the inlet, the collection is stopped, and 40mL of pricklyash seed oil is collected. The final phosphorus content was 58.4 ppm.
Example 4
Sulfonic acid type cationic resin Amberlite FPC11+ hydration dephosphorization experiment for rapeseed crude oil dephosphorization
Adding 25mL of rapeseed crude oil (phosphorus content: 384.2ppm) into a shake flask, adding softened hot water of 5% vol and 80 deg.C into the oil phase, and shaking at 80 deg.C and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain oil subjected to hydration dephosphorization. Then 20mL of supernatant oil is taken, and 1g of functional group is-SO3H Amberlite FPC11 resin (Rohm and Haas, USA). The shake flask was placed in a shaker and shaken at 60 ℃ at a constant temperature of 200r/min for 6 h. Then taking out the oil phase, adding softened hot water with the pH value of 8.0 at 80 ℃ and 5% vol into the oil phase, and shaking at the constant temperature of 80 ℃ and 200r/min for 30 min; and centrifuging at 8000r/min for 20min to obtain refined oil.
The final phosphorus content after treatment by this method was 6.5 ppm.
Claims (5)
1. A grease dephosphorization method with cationic resin is characterized in that grease to be treated is fully contacted with strong acid cationic resin, and phospholipid of the treated grease is removed by a hydration dephosphorization method to obtain dephosphorized grease;
wherein the functional group of the strong acid cation resin is-SO3H；
The full contact is that the grease to be treated is directly mixed with the strong acid cation resin, or the grease to be treated flows through a column filled with the strong acid cation resin;
directly mixing the grease with the strong acid cation resin, and specifically operating as follows:
adding strong acid cation resin with the mass of 1-10% of that of the grease into the grease to be treated, and shaking for 5-8 h in a shaking table at constant temperature at 60 ℃ and 200 r/min;
the grease to be treated flows through a column filled with strong acid cation resin, and the specific operation is as follows:
the grease to be treated was continuously passed through a column packed with a strongly acidic cation resin at a flow rate of 1BV/h, and the effluent was collected at the outlet of the column.
2. Process for the cationic resin dephosphorization of fats & oils according to claim 1, wherein said collection operation is ended when calcium ions are leaked out in the effluent and less than 5 ppm.
3. Process for the dephosphorization of cationic resins of fats & oils according to claim 1, wherein said strongly acidic cationic resins are capable of regeneration, the regeneration process comprising the following steps:
1) using distilled water with the volume of 2BV to pass through the column to replace grease in the column, wherein the flow rate is 1BV/h, and the flow direction is from bottom to top;
2) using 2-2.5 BV H10% by volume2SO4Enabling the solution to flow through the column at the flow rate of 2BV/h and in the flow direction from bottom to top;
3) passing distilled water with the volume of 2BV through the column at the flow rate of 2BV/h in the flow direction from top to bottom;
4) 2BV of refined oil is used for passing through the column, the water in the column is replaced, the flow rate is 2BV/h, and the flow direction is from top to bottom.
4. The method for dephosphorization of grease with cationic resin according to any one of claims 1 to 3, wherein said method for hydration dephosphorization is to add softened hot water which occupies 5% of the grease volume, 80 ℃ and pH value of 5 to 8 to grease treated with strong acid cationic resin, shake in a shaker at 80 ℃ to 85 ℃ and 200r/min for 20min to 45min at constant temperature, and centrifuge at 8000r/min for 20 min.
5. The method for dephosphorizing by cationic resin of oil and fat according to any one of claims 1 to 3, wherein said oil and fat to be treated is subjected to hydration dephosphorization treatment before being fully contacted with strong acidic cationic resin.
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