CN113150863A - Method for reducing anisidine value of grease by adopting macroporous adsorption resin - Google Patents
Method for reducing anisidine value of grease by adopting macroporous adsorption resin Download PDFInfo
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- CN113150863A CN113150863A CN202110155924.9A CN202110155924A CN113150863A CN 113150863 A CN113150863 A CN 113150863A CN 202110155924 A CN202110155924 A CN 202110155924A CN 113150863 A CN113150863 A CN 113150863A
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- resin
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- 239000011347 resin Substances 0.000 title claims abstract description 92
- 229920005989 resin Polymers 0.000 title claims abstract description 92
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 65
- 239000004519 grease Substances 0.000 title claims abstract description 57
- BHAAPTBBJKJZER-UHFFFAOYSA-N p-anisidine Chemical compound COC1=CC=C(N)C=C1 BHAAPTBBJKJZER-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 238000001514 detection method Methods 0.000 claims abstract description 8
- 238000007865 diluting Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 60
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 12
- 239000003463 adsorbent Substances 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 239000003638 chemical reducing agent Substances 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 5
- 238000012512 characterization method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 19
- 239000003921 oil Substances 0.000 description 12
- 235000019198 oils Nutrition 0.000 description 12
- 239000007788 liquid Substances 0.000 description 6
- 238000002390 rotary evaporation Methods 0.000 description 6
- 238000010998 test method Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000000944 linseed oil Substances 0.000 description 3
- 235000021388 linseed oil Nutrition 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 240000004308 marijuana Species 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- CMVHOLZLFLESKY-UHFFFAOYSA-N Anisodine Natural products CN1C2CC(CC1C3OC23)C(=O)OC(O)(CO)c4ccccc4 CMVHOLZLFLESKY-UHFFFAOYSA-N 0.000 description 1
- JEJREKXHLFEVHN-QDXGGTILSA-N anisodine Chemical compound C1([C@](O)(CO)C(=O)OC2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 JEJREKXHLFEVHN-QDXGGTILSA-N 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010460 hemp oil Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
Classifications
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a method for reducing the anisidine value of grease by adopting macroporous adsorption resin, which comprises the following steps: diluting the grease with a solvent, performing dynamic adsorption by using macroporous adsorption resin, and collecting the effluent until the detection reaches the upper limit of a required value; and removing the solvent from the collected effluent to obtain the treated grease. Compared with the prior art, the method adopts macroporous adsorption resin to continuously flow and adsorb to reduce the anisidine value of the grease, and effectively solves the problem of the anisidine value rise caused by secondary processing, storage and the like of the grease in the production process of the grease; the macroporous adsorption resin has the advantages of selective adsorption, simple equipment, simple operation, low production and operation cost, high efficiency of removing the anisidine value characterization object, no secondary pollution to products, recycling, and wide application in the grease industry compared with the traditional intermittent treatment method using a reducing agent.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a method for reducing an anisidine value of grease by adopting macroporous adsorption resin.
Background
In the production process and the storage process of the grease, the grease is easily subjected to secondary oxidation due to the influence of a plurality of factors such as temperature, illumination and the like. The existing method for reducing the peroxide value of the grease is to remove the grease by adopting activated carbon vacuum high-temperature adsorption, intermittent operation is carried out, the grease loss is large, the anisidine value of the grease is increased after secondary high-temperature treatment, and after the peroxide value reaches the index requirement, the anisidine value is increased, namely a primary oxidation product of the grease is converted into a secondary oxidation product, so that the grease quality is greatly reduced.
The prior patent discloses that a reducing agent can be used for reducing the anisidine value, but the method cannot be realized in actual production at all, and a great number of reducing agents are chemical reagents and cannot meet the requirements of food production, so that the treatment of the anisidine value becomes a difficult problem in the oil industry.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for reducing the anisidine value of oil by using macroporous adsorption resin, which can be performed in a linked manner, effectively solves the quality problem caused by the secondary oxidation of oil in the oil industry, and has the advantages of safer and more reliable treatment effect and greatly improved product quality.
The invention provides a method for reducing the anisidine value of grease by adopting macroporous adsorption resin, which comprises the following steps:
diluting the grease with a solvent, performing dynamic adsorption by using macroporous adsorption resin, and collecting the effluent until the detection reaches the upper limit of a required value;
and removing the solvent from the collected effluent to obtain the treated grease.
Preferably, the solvent is n-hexane; the mass concentration of the grease in the diluted solution is 30-50%.
Preferably, the macroporous adsorption resin is weak-polarity macroporous adsorption resin.
Preferably, the macroporous adsorption resin is activated and then dynamically adsorbed;
the activation treatment specifically comprises the following steps:
soaking macroporous adsorption resin in desalted water, loading the macroporous adsorption resin into a column by using hydrochloric acid, washing the macroporous adsorption resin with desalted water until the pH value of an effluent is more than 3, loading the effluent into the column by using a sodium hydroxide solution, washing the effluent by using the desalted water until the conductivity of the effluent is less than 30us/cm, and finally sequentially replacing water in the resin by using ethanol and normal hexane.
Preferably, the volume of the hydrochloric acid is 1.5-2.5 BV of the volume of the resin when the hydrochloric acid is filled into the column; the flow rate of the hydrochloric acid in column filling is 0.5-1.5 BV/h.
Preferably, the concentration of the sodium hydroxide solution is 4-8%; the flow rate of the sodium hydroxide solution is 0.5-1.5 BV/h; the volume of the sodium hydroxide solution is 1.5-2.5 BV of the volume of the resin.
Preferably, the flow rate of the ethanol is 0.5-1.5 BV/h; the volume of the ethanol is 1.5-2.5 BV of the volume of the resin;
the flow rate of the normal hexane is 0.5-1.5 BV/h; the volume of the n-hexane is 1.5-2.5 BV of the volume of the resin.
Preferably, the volume of the hydrochloric acid is 2BV of the resin volume when the hydrochloric acid is filled into the column; the flow rate of hydrochloric acid in column filling is 1 BV/h;
the concentration of the sodium hydroxide solution is 5%; the flow rate of the sodium hydroxide solution is 1 BV/h; the volume of the sodium hydroxide solution is 2BV of the resin volume;
the flow rate of the ethanol is 1 BV/h; the volume of the ethanol is 2BV of the volume of the resin;
the flow rate of the n-hexane is 1 BV/h; the volume of the n-hexane is 2BV of the resin volume.
Preferably, the temperature of the dynamic adsorption is 30-50 ℃.
Preferably, the retention time of the diluted grease in the macroporous adsorption resin is 0.5-3 h; the flow speed of the diluted grease during dynamic adsorption is 0.3-0.5 BV/h.
The invention provides a method for reducing the anisidine value of grease by adopting macroporous adsorption resin, which comprises the following steps: diluting the grease with a solvent, performing dynamic adsorption by using macroporous adsorption resin, and collecting the effluent until the detection reaches the upper limit of a required value; and removing the solvent from the collected effluent to obtain the treated grease. Compared with the prior art, the method adopts macroporous adsorption resin to continuously flow and adsorb to reduce the anisidine value of the grease, and effectively solves the problem of the anisidine value rise caused by secondary processing, storage and the like of the grease in the production process of the grease; the macroporous adsorption resin has the advantages of selective adsorption, simple equipment, simple operation, low production and operation cost, high efficiency of removing the anisidine value characterization object, no secondary pollution to products, recycling, and wide application in the grease industry compared with the traditional intermittent treatment method using a reducing agent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for reducing the anisidine value of grease by adopting macroporous adsorption resin, which comprises the following steps: diluting the grease with a solvent, performing dynamic adsorption by using macroporous adsorption resin, and collecting the effluent until the detection reaches the upper limit of a required value; and removing the solvent from the collected effluent to obtain the treated grease.
In the present invention, the sources of all raw materials are not particularly limited, and they may be commercially available.
Diluting the grease with a solvent; the grease can be vegetable grease or animal grease, and is not particularly limited, and in the embodiment provided by the invention, the grease is specifically linseed oil or hemp oil; the solvent is preferably n-hexane; the mass concentration of the grease in the diluted solution is preferably 30-50%; in the embodiment provided by the invention, the mass concentration of the grease in the diluted solution is 30% or 50%.
Dynamically adsorbing the diluted solution by using macroporous adsorption resin; the macroporous adsorption resin is preferably weak-polarity macroporous adsorption resin, and more preferably LSA series resin; in the embodiment provided by the invention, the macroporous adsorption resin is specifically LSA-900D; the macroporous adsorption resin is preferably subjected to activation treatment and then dynamic adsorption; the activation treatment specifically comprises the following steps: soaking macroporous adsorption resin in desalted water, loading the macroporous adsorption resin into a column by using hydrochloric acid, washing the macroporous adsorption resin with desalted water until the pH value of an effluent is more than 3, loading the effluent into the column by using a sodium hydroxide solution, washing the effluent by using the desalted water until the conductivity of the effluent is less than 30us/cm, and finally sequentially replacing water in the resin by using ethanol and normal hexane. The soaking time of the desalted water is preferably more than 24 hours; the concentration of the hydrochloric acid is preferably 5% v/v to 10% v/v, and more preferably 7% v/v; the volume of the hydrochloric acid is preferably 1.5-2.5 BV, more preferably 1.8-2.2 BV, and even more preferably 2BV of the resin volume when the hydrochloric acid is filled into the column; the flow rate of the hydrochloric acid in column filling is preferably 0.5-1.5 BV/h, more preferably 0.8-1.2 BV/h, and still more preferably 1 BV/h; the mass concentration of the sodium hydroxide solution is preferably 4-8%, and more preferably 5-6%; the flow rate of the sodium hydroxide solution is preferably 0.5-1.5 BV/h, more preferably 0.8-1.2 BV/h, and still more preferably 1 BV/h; the volume of the sodium hydroxide solution is preferably 1.5-2.5 BV of the resin volume, more preferably 1.8-2.2 BV, and still more preferably 2 BV; the concentration of the ethanol is preferably 95%; the flow rate of the ethanol is preferably 0.5-1.5 BV/h, more preferably 0.8-1.2 BV/h, and still more preferably 1 BV/h; the volume of the ethanol is preferably 1.5-2.5 BV of the volume of the resin, more preferably 1.8-2.2 BV, and still more preferably 2 BV; the flow rate of the normal hexane is preferably 0.5-1.5 BV/h, more preferably 0.8-1.2 BV/h, and still more preferably 1 BV/h; the volume of the n-hexane is preferably 1.5-2.5 BV, more preferably 1.8-2.2 BV and even more preferably 2BV of the resin volume; the temperature of the dynamic adsorption is preferably 30-50 ℃, and more preferably 40-50 ℃; in the embodiment provided by the invention, the temperature of the dynamic adsorption is specifically 50 ℃; during dynamic adsorption, the flow speed of the diluted grease is preferably 0.3-0.5 BV/h; the residence time of the diluted grease in the macroporous adsorption resin is preferably 0.5-3 h, more preferably 0.5-2 h, and still more preferably 0.5-1 h.
And dynamically adsorbing and collecting the effluent until the detection reaches the upper limit of the required value, and stopping collecting the effluent. The macroporous adsorption resin after adsorption can be recycled after the activation treatment; in the invention, the used macroporous adsorption resin is preferably prepared by firstly using normal hexane to replace residual oil in the resin, then sequentially using ethanol and desalted water to wash the residual oil, and then performing the activation treatment for recycling; the volume of the n-hexane is preferably 1.5-2.5 BV, more preferably 1.8-2.2 BV and even more preferably 2BV of the resin volume; the volume of the ethanol used for washing is preferably 1.5-2.5 BV of the volume of the resin, more preferably 1.8-2.2 BV, and still more preferably 2 BV; the volume of the desalted water used for washing is 0.5-1.5 BV, more preferably 0.8-1.2 BV, and still more preferably 1BV of the resin volume.
Removing the solvent from the collected effluent to obtain treated grease; in the present invention, the solvent is preferably removed by rotary evaporation; the rotary evaporation temperature is preferably 65-110 ℃, and more preferably 80-110 ℃; the solvent removed by rotary evaporation can also be recovered for reuse.
The invention adopts macroporous adsorption resin to continuously flow and adsorb to reduce the anisidine value of the grease, thereby effectively solving the problem of the anisidine value rise caused by secondary processing, storage and the like of the grease in the production process of the grease; the macroporous adsorption resin has the advantages of selective adsorption, simple equipment, simple operation, low production and operation cost, high efficiency of removing the anisidine value characterization object, no secondary pollution to products, recycling, and wide application in the grease industry compared with the traditional intermittent treatment method using a reducing agent.
In order to further illustrate the present invention, the following will describe in detail a method for reducing the anisidine value of grease by using macroporous adsorbent resin according to the present invention with reference to the examples.
The reagents used in the following examples are all commercially available.
The macroporous adsorbent resin LSA-900D was purchased from Xian blue Xiao science and technology Co. Before use, activation treatment is needed, and the method comprises the following specific steps: soaking the macroporous adsorption resin in desalted water for more than 24 hours, loading the macroporous adsorption resin on a column by hydrochloric acid with the volume of 7% v/v of 2BV of the resin at the flow rate of 1BV/h, washing the macroporous adsorption resin with desalted water until the pH of the effluent is more than 3, configuring a sodium hydroxide column with the volume of 5%, the flow rate of 1BV/h and the total volume of 2BV, washing the effluent with the desalted water until the conductivity of the effluent is less than 30us/cm, finally loading the effluent on the column by 95% ethanol at the flow rate of 1BV/h and the total volume of 2BV, loading the effluent on the column by n-hexane at the flow rate of 1BV/h and the total volume of 2BV for later use.
Example 1
Preparing linseed oil with anisidine value of 23.39(GBT24304-2009 test method), diluting with n-hexane to concentration of 30% to obtain a column loading solution, loading the column loading activated macroporous adsorption resin, keeping the temperature of the resin column at 50 ℃ and the flow rate at 0.3BV/h, collecting effluent liquid, detecting, stopping collecting the effluent liquid when the detection result is more than 15, carrying out rotary evaporation on the collection liquid at 110 ℃, and recovering the n-hexane to obtain the treated grease.
The anisidine value of the treated oil is detected according to a test method of GBT24304-2009, the resin effectively adsorbs for 48 hours, the anisidine value of the mixed solution is 10.20, and the anisidine value is reduced by 56%.
Example 2
Preparing cannabis oil with an anisidine value of 25.42(GBT24304-2009 test method), diluting the cannabis oil with n-hexane to reach a concentration of 50% to obtain a column loading solution, loading the column loading activated macroporous adsorbent resin, keeping the temperature of the resin column at 50 ℃ and the flow rate at 0.5BV/h, collecting and detecting the effluent, stopping collecting the effluent when the detection result is more than 15, carrying out rotary evaporation on the collected solution at 110 ℃, and recovering the n-hexane to obtain the treated oil.
The anisidine value of the treated grease is detected according to a GBT24304-2009 test method, the resin effectively adsorbs for 36 hours, the anisidine value of the mixed solution is 11.28, and the anisidine value is reduced by 55.6%.
Example 3
The resin used in example 1 was regenerated. The regeneration method comprises the following steps: firstly, 2BV of n-hexane is used for completely displacing residual oil in the resin; then 2BV of ethanol and 1BV of desalted water. Soaking macroporous adsorbent resin in desalted water for more than 24 hours, loading the macroporous adsorbent resin in hydrochloric acid with the volume of 7% v/v of 2BV of the resin on a column at the flow rate of 1BV/h, washing the macroporous adsorbent resin with desalted water until the pH of the effluent is more than 3, preparing a sodium hydroxide upper column with the volume of 5%, the flow rate of 1BV/h and the total volume of 2BV, washing the effluent with desalted water until the conductivity of the effluent is less than 30us/cm, loading the effluent on the column with 95% ethanol at the flow rate of 1BV/h and the total volume of 2BV, loading the effluent on a column with n-hexane at the flow rate of 1BV/h and the total volume of 2BV for later use
Preparing 50% linseed oil (anisodine value of raw material is 27.53) with n-hexane to obtain upper column liquid with flow rate of 0.5BV/h, collecting liquid, performing rotary evaporation on the collected liquid at 110 ℃, and recovering n-hexane to obtain the treated oil. And detecting the treated anisidine value according to a GBT24304-2009 test method. The results are shown in Table 1. The effective service life of the regenerated resin is about 36 hours, the anisidine value of the mixed solution is 12.18, and is reduced by 56 percent compared with the anisidine value of the raw material. The service life of the resin is 2-3 years.
Table 1 example 3 resin recycling test results
| Cumulative hour/h | Flow rate BV/h | P-A |
| 1 | 0.5 | 8.82 |
| 3 | 0.5 | 9.45 |
| 5 | 0.5 | 9.67 |
| 7 | 0.5 | 9.97 |
| 9 | 0.5 | 10.08 |
| 11 | 0.5 | 10.34 |
| 13 | 0.5 | 10.54 |
| 15 | 0.5 | 11.23 |
| 17 | 0.5 | 11.36 |
| 19 | 0.5 | 11.89 |
| 21 | 0.5 | 12.04 |
| 23 | 0.5 | 12.54 |
| 25 | 0.5 | 12.99 |
| 27 | 0.5 | 13.18 |
| 29 | 0.5 | 13.67 |
| 31 | 0.5 | 14.10 |
| 33 | 0.5 | 14.57 |
| 35 | 0.5 | 14.78 |
| 37 | 0.5 | 15.37 |
| Mixed sample | 12.18 |
Claims (10)
1. A method for reducing the anisidine value of grease by adopting macroporous adsorption resin is characterized by comprising the following steps:
diluting the grease with a solvent, performing dynamic adsorption by using macroporous adsorption resin, and collecting the effluent until the detection reaches the upper limit of a required value;
and removing the solvent from the collected effluent to obtain the treated grease.
2. The method of claim 1, wherein the solvent is n-hexane; the mass concentration of the grease in the diluted solution is 30-50%.
3. The method of claim 1, wherein the macroporous adsorbent resin is a weakly polar macroporous adsorbent resin.
4. The method according to claim 1, wherein the macroporous adsorbent resin is activated and then subjected to dynamic adsorption;
the activation treatment specifically comprises the following steps:
soaking macroporous adsorption resin in desalted water, loading the macroporous adsorption resin into a column by using hydrochloric acid, washing the macroporous adsorption resin with desalted water until the pH value of an effluent is more than 3, loading the effluent into the column by using a sodium hydroxide solution, washing the effluent by using the desalted water until the conductivity of the effluent is less than 30us/cm, and finally sequentially replacing water in the resin by using ethanol and normal hexane.
5. The method according to claim 4, wherein the volume of the hydrochloric acid in column packing is 1.5-2.5 BV; the flow rate of the hydrochloric acid in column filling is 0.5-1.5 BV/h.
6. The method according to claim 4, wherein the concentration of the sodium hydroxide solution is 4% to 8%; the flow rate of the sodium hydroxide solution is 0.5-1.5 BV/h; the volume of the sodium hydroxide solution is 1.5-2.5 BV of the volume of the resin.
7. The method according to claim 4, wherein the flow rate of the ethanol is 0.5-1.5 BV/h; the volume of the ethanol is 1.5-2.5 BV of the volume of the resin;
the flow rate of the normal hexane is 0.5-1.5 BV/h; the volume of the n-hexane is 1.5-2.5 BV of the volume of the resin.
8. The method of claim 4, wherein the volume of hydrochloric acid in the column is 2 BV; the flow rate of hydrochloric acid in column filling is 1 BV/h;
the concentration of the sodium hydroxide solution is 5%; the flow rate of the sodium hydroxide solution is 1 BV/h; the volume of the sodium hydroxide solution is 2BV of the resin volume;
the flow rate of the ethanol is 1 BV/h; the volume of the ethanol is 2BV of the volume of the resin;
the flow rate of the n-hexane is 1 BV/h; the volume of the n-hexane is 2BV of the resin volume.
9. The method of claim 1, wherein the temperature of the dynamic adsorption is from 30 ℃ to 50 ℃.
10. The method according to claim 1, wherein the retention time of the diluted grease in the macroporous adsorption resin is 0.5-3 h; the flow speed of the diluted grease during dynamic adsorption is 0.3-0.5 BV/h.
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