CN115531914A - Wet meal desolventizing method - Google Patents
Wet meal desolventizing method Download PDFInfo
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- CN115531914A CN115531914A CN202211169387.4A CN202211169387A CN115531914A CN 115531914 A CN115531914 A CN 115531914A CN 202211169387 A CN202211169387 A CN 202211169387A CN 115531914 A CN115531914 A CN 115531914A
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- biochar
- wet meal
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- wet
- cottonseed
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- 235000012054 meals Nutrition 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 37
- 235000012343 cottonseed oil Nutrition 0.000 claims abstract description 70
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003463 adsorbent Substances 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000011347 resin Substances 0.000 claims abstract description 27
- 239000011230 binding agent Substances 0.000 claims abstract description 18
- 238000004821 distillation Methods 0.000 claims abstract description 17
- 235000017060 Arachis glabrata Nutrition 0.000 claims abstract description 15
- 235000010777 Arachis hypogaea Nutrition 0.000 claims abstract description 15
- 235000018262 Arachis monticola Nutrition 0.000 claims abstract description 15
- 239000004793 Polystyrene Substances 0.000 claims abstract description 15
- 239000003822 epoxy resin Substances 0.000 claims abstract description 15
- 235000020232 peanut Nutrition 0.000 claims abstract description 15
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 15
- 229920002223 polystyrene Polymers 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000019441 ethanol Nutrition 0.000 claims abstract description 10
- -1 biochar Substances 0.000 claims abstract description 8
- 241001553178 Arachis glabrata Species 0.000 claims abstract 2
- 239000002245 particle Substances 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- GCFHZZWXZLABBL-UHFFFAOYSA-N ethanol;hexane Chemical compound CCO.CCCCCC GCFHZZWXZLABBL-UHFFFAOYSA-N 0.000 claims description 7
- 238000007710 freezing Methods 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- 241000196324 Embryophyta Species 0.000 claims description 4
- 238000005336 cracking Methods 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- QBKSWRVVCFFDOT-UHFFFAOYSA-N gossypol Chemical compound CC(C)C1=C(O)C(O)=C(C=O)C2=C(O)C(C=3C(O)=C4C(C=O)=C(O)C(O)=C(C4=CC=3C)C(C)C)=C(C)C=C21 QBKSWRVVCFFDOT-UHFFFAOYSA-N 0.000 abstract description 22
- QHOPXUFELLHKAS-UHFFFAOYSA-N Thespesin Natural products CC(C)c1c(O)c(O)c2C(O)Oc3c(c(C)cc1c23)-c1c2OC(O)c3c(O)c(O)c(C(C)C)c(cc1C)c23 QHOPXUFELLHKAS-UHFFFAOYSA-N 0.000 abstract description 11
- 229930000755 gossypol Natural products 0.000 abstract description 11
- 229950005277 gossypol Drugs 0.000 abstract description 11
- 239000002904 solvent Substances 0.000 abstract description 11
- 241001465754 Metazoa Species 0.000 abstract description 6
- 235000019198 oils Nutrition 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 26
- 244000105624 Arachis hypogaea Species 0.000 description 13
- 229920000742 Cotton Polymers 0.000 description 11
- 239000000853 adhesive Substances 0.000 description 11
- 230000001070 adhesive effect Effects 0.000 description 11
- 229920002635 polyurethane Polymers 0.000 description 7
- 239000004814 polyurethane Substances 0.000 description 7
- 239000003522 acrylic cement Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000019750 Crude protein Nutrition 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 239000002385 cottonseed oil Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 229920005822 acrylic binder Polymers 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
- A23K10/37—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms from waste material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Molecular Biology (AREA)
- Mycology (AREA)
- Physiology (AREA)
- Animal Husbandry (AREA)
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Abstract
The invention relates to the technical field of oil processing, and discloses a wet meal desolventizing method, which comprises the steps of adding absolute ethyl alcohol into wet meal raw materials, vibrating and dispersing the absolute ethyl alcohol, distilling the wet meal raw materials, and adsorbing steam obtained by distillation by using a biochar-resin adsorbent to obtain desolventized wet meal; specifically, the biochar-resin adsorbent consists of water, biochar, epoxy resin, polystyrene and a binder, wherein the biochar is cottonseed hulls and/or peanut hulls; by utilizing the wet meal desolventizing method disclosed by the invention, the n-hexane solvent and free gossypol can be effectively removed, so that the desolventized cottonseed meal meets the national standard; meanwhile, the wet meal raw material is treated by using the ethanol, so that the wet meal can be effectively sterilized, and the wet meal obtained by exsolution can be directly used for preparing animal feed.
Description
Technical Field
The invention relates to the technical field of oil processing, in particular to a wet meal desolventizing method.
Background
The cotton has the characteristics of high yield, low production cost and the like, so the cotton is one of the main crops in the world. The cottonseed is the seed of cotton, which is the main vegetable oil next to soybean, and the cottonseed kernel obtained after delinting and shelling the cottonseed is the raw material for preparing the cottonseed oil. The residual granular material after the cottonseed oil is prepared by using cottonseed kernels is cottonseed meal which contains more than 40 percent of crude protein and is a main raw material for preparing animal feed.
The crude oil extraction from the cottonseed kernels comprises three modes of hydraulic pressure, spinning and solvent extraction, wherein the solution extraction method is used frequently. N-hexane is a colorless liquid, belongs to straight-chain saturated aliphatic hydrocarbon, and is mainly used as a solvent, a chromatographic analysis reference substance, a coating diluent, a polymerization reaction medium and the like. Currently in the grease processing industry, n-hexane is the most predominant solvent for vegetable oil leaching. Although most of the solvent is removed by the production processes such as distillation and the like in the production process of the oil, a small amount of n-hexane solvent remains in the cottonseed meal. For animals, n-hexane is a low-toxicity substance, and when the residual solubility in the cottonseed meal feed exceeds the standard, the animals can be damaged and even die.
Therefore, an effective cottonseed meal desolventizing method is needed to effectively reduce the content of the n-hexane solvent in the cottonseed meal and improve the utilization rate and the utilization value of the cottonseed meal.
Disclosure of Invention
In order to solve the technical problem, the invention provides a wet meal desolventizing method, which comprises the following steps:
adding absolute ethyl alcohol into the wet meal raw material, oscillating and dispersing, distilling, and adsorbing steam obtained by distillation by using an adsorbent to obtain desolventized wet meal;
wherein the adsorbent is a biochar-resin adsorbent.
Further, the wet meal raw material is frozen and crushed to obtain cottonseed meal particles, and then absolute ethyl alcohol is added into the cottonseed meal particles for vibration dispersion.
Further, the addition amount of the absolute ethyl alcohol is 20-30% of the weight of the wet meal raw material.
Further, the grain size of the cottonseed meal particles is 50-200 meshes.
Further, the temperature of the distillation is 67-80 ℃.
Further, the preparation method of the biochar-resin adsorbent comprises the following steps:
uniformly mixing water, biochar, epoxy resin, polystyrene and a binder, plasticizing for 2-4h under a vacuum condition, and drying to obtain the biochar-resin adsorbent.
Further, the weight part ratio of the water, the biochar, the epoxy resin, the polystyrene, the flow assistant and the binder is 9-13:65-70:8-15:3-5:3-6.
further, the adhesive is an acrylic adhesive and/or a polyurethane adhesive.
Further, when the adhesive is an acrylic adhesive and a polyurethane adhesive, the weight part ratio of the acrylic adhesive to the polyurethane adhesive is 1-2:1-2.
further, the preparation method of the biochar comprises the following steps:
pulverizing plant-based raw materials into powder with particle size of 100-200 mesh, cracking at high temperature under the conditions of room temperature, uniformly heating to 500-600 deg.C at a speed of 8-12 deg.C/min, maintaining for 2-4 hr, introducing CO 2 Activating for 0.5-1h, and then cooling to room temperature at a constant speed of 16-20 ℃/min to obtain the biochar.
Further, the plant-based raw material is cottonseed hull and/or peanut hull.
Further, the steam is ethanol steam, n-hexane steam and/or ethanol-n-hexane azeotropic steam.
Compared with the prior art, its beneficial effect lies in:
the invention provides a wet meal desolventizing method, which comprises the steps of adding absolute ethyl alcohol into wet meal raw materials, vibrating and dispersing the materials, distilling the materials, and adsorbing steam obtained by distillation by using a charcoal-resin adsorbent to obtain desolventized wet meal; specifically, the biochar-resin adsorbent consists of water, biochar, epoxy resin, polystyrene and a binder, wherein the biochar is cottonseed hulls and/or peanut hulls; by utilizing the wet meal desolventizing method disclosed by the invention, the n-hexane solvent and free gossypol can be effectively removed, so that the desolventized cottonseed meal meets the national standard; meanwhile, the wet meal raw material is treated by using the ethanol, so that the wet meal can be effectively sterilized, and the wet meal obtained by exsolution can be directly used for preparing animal feed.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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 wet meal used in the following examples is cottonseed wet meal comprising n-hexane solvent.
Example 1
The embodiment provides a preparation method of biochar, which comprises the following steps:
crushing cottonseed hulls into powder with the particle size of 200 meshes, and carrying out pyrolysis by using a muffle furnace under the specific conditions: the initial temperature is room temperature, the temperature is raised to 600 ℃ at a constant speed of 10 ℃/min, the temperature is kept for 4h, the cotton seed hull biochar is obtained after being cooled to room temperature at a constant speed of 20 ℃/min and then screened by a 200-mesh sieve.
Example 2
The embodiment provides a preparation method of biochar, which comprises the following steps:
crushing peanut shell into powder with the particle size of 150 meshes, and performing pyrolysis by using a muffle furnace under the specific conditions that: the initial temperature is room temperature, the temperature is raised to 550 ℃ at a constant speed of 8 ℃/min, the temperature is maintained for 3h, the cotton seed hull biochar is obtained after being cooled to room temperature at a constant speed of 18 ℃/min and sieved by a 150-mesh sieve.
Example 3
The embodiment provides a preparation method of biochar, which comprises the following steps:
crushing cottonseed hulls and peanut hulls into powder with the particle size of 150 meshes, and mixing the cottonseed hulls powder and the peanut hulls powder according to the weight ratio of 1:3, and carrying out pyrolysis by using a muffle furnace, wherein the specific conditions are as follows: the initial temperature is room temperature, the temperature is raised to 500 ℃ at a constant speed of 12 ℃/min, the temperature is maintained for 2h, the cotton seed hull-peanut hull charcoal A is obtained after the cotton seed hull-peanut hull charcoal is cooled to room temperature at a constant speed of 15 ℃/min and is sieved by a 150-mesh sieve.
Example 4
The embodiment provides a preparation method of biochar, which comprises the following steps:
crushing cottonseed hulls and peanut hulls into powder with the particle size of 200 meshes, and taking the cottonseed hulls powder and the peanut hulls powder according to the following weight parts of 3:1, carrying out pyrolysis by using a muffle furnace, wherein the specific conditions are as follows: the initial temperature is room temperature, the temperature is raised to 550 ℃ at a constant speed of 10 ℃/min, the temperature is maintained for 3h, the cotton seed hull-peanut hull biochar B is obtained after the cotton seed hull-peanut hull biochar B is cooled to room temperature at a constant speed of 20 ℃/min and is sieved by a 200-mesh sieve.
Example 5
The embodiment provides a preparation method of biochar, which comprises the following steps:
crushing cottonseed hulls and peanut hulls into powder with the particle size of 100 meshes, and mixing the cottonseed hulls powder and the peanut hulls powder according to the weight ratio of 1:1, carrying out pyrolysis by using a muffle furnace, wherein the specific conditions are as follows: the initial temperature is room temperature, the temperature is raised to 600 ℃ at a constant speed of 10 ℃/min, the temperature is kept for 4h, the cotton seed hull-peanut hull biochar C is obtained after the cotton seed hull-peanut hull biochar C is cooled to room temperature at a constant speed of 18 ℃/min and is sieved by a 100-mesh sieve.
Example 6
The embodiment provides a preparation method of a biochar-resin adsorbent, which comprises the following steps:
the weight portion ratio is 13:70:15:5:6, uniformly mixing water, the biochar, the epoxy resin, the polystyrene and the binder, plasticizing for 3.5 hours under a vacuum condition, and drying to obtain the biochar-resin adsorbent A; specifically, the biochar is the cottonseed hull biochar prepared in example 1; the binder is a polyurethane binder.
Example 7
The embodiment provides a preparation method of a biochar-resin adsorbent, which comprises the following steps:
the weight portion ratio is 9:65:8:3:3, uniformly mixing water, the biochar, the epoxy resin, the polystyrene and the binder, plasticizing for 2 hours under a vacuum condition, and drying to obtain the biochar-resin adsorbent B; specifically, the biochar is the peanut shell biochar prepared in example 2; the binder is an acrylic binder.
Example 8
The embodiment provides a preparation method of a biochar-resin adsorbent, which comprises the following steps:
the weight portion ratio is 13:70:15:5:6, uniformly mixing water, the biochar, the epoxy resin, the polystyrene and a binder, plasticizing for 2.5 hours under a vacuum condition, and drying to obtain a biochar-resin adsorbent C; specifically, the biochar is the cottonseed hull-peanut hull biochar a prepared in example 3; the adhesive is an acrylic adhesive and a polyurethane adhesive, and the weight part ratio is 1:1.
example 9
The embodiment provides a preparation method of a biochar-resin adsorbent, which comprises the following steps:
the weight portion ratio is 9:65:8:3:3, uniformly mixing water, the biochar, the epoxy resin, the polystyrene and the binder, plasticizing for 3 hours under a vacuum condition, and drying to obtain the biochar-resin adsorbent D; specifically, the biochar is the cottonseed hull-peanut hull biochar B prepared in example 3; the adhesive is an acrylic adhesive and a polyurethane adhesive, and the weight part ratio is 2:1.
example 10
The embodiment provides a preparation method of a biochar-resin adsorbent, which comprises the following steps:
the weight portion ratio is 11:68:12:4:4, uniformly mixing water, the biochar, the epoxy resin, the polystyrene and the binder, plasticizing for 4 hours under a vacuum condition, and drying to obtain the biochar-resin adsorbent E; specifically, the biochar is the cottonseed hull-peanut hull biochar C prepared in example 3; the adhesive is an acrylic adhesive and a polyurethane adhesive, and the weight part ratio is 1:2.
example 11
The embodiment provides a wet meal desolventizing method, which comprises the following steps:
freezing a cottonseed wet meal raw material at a temperature lower than zero degree, crushing the frozen cottonseed wet meal raw material into powder with the particle size of 200 meshes to obtain cottonseed meal particles, adding anhydrous ethanol with the weight of 20% of the weight of the cottonseed meal particles into the cottonseed meal particles, oscillating and dispersing the mixture, distilling the mixture at 78 ℃, adsorbing steam obtained by distillation by using the biochar-resin adsorbent A prepared in example 6, and obtaining desolventized wet meal A; specifically, the steam is ethanol steam, n-hexane steam and ethanol-n-hexane azeotropic steam.
Example 12
The embodiment provides a wet meal desolventizing method, which comprises the following steps:
freezing a cottonseed wet meal raw material at a temperature lower than zero degree, crushing the frozen cottonseed wet meal raw material into powder with the particle size of 50 meshes to obtain cottonseed meal particles, adding absolute ethyl alcohol with the weight of 30% of the weight of the cottonseed meal particles into the cottonseed meal particles, oscillating and dispersing the absolute ethyl alcohol, distilling the mixture at 73 ℃, and adsorbing steam obtained by distillation by using the biochar-resin adsorbent B prepared in example 7 to obtain desolventized wet meal B; specifically, the steam is ethanol steam, n-hexane steam and ethanol-n-hexane azeotropic steam.
Example 13
The embodiment provides a wet meal desolventizing method, which comprises the following steps:
freezing a cottonseed wet meal raw material at a temperature lower than zero degree, crushing the frozen cottonseed wet meal raw material into powder with the particle size of 100 meshes to obtain cottonseed meal particles, adding absolute ethyl alcohol with the weight of 25% of the weight of the cottonseed meal particles into the cottonseed meal particles, oscillating and dispersing the absolute ethyl alcohol, distilling the mixture at 70 ℃, adsorbing steam obtained by distillation by using the charcoal-resin adsorbent C prepared in the embodiment 8, and obtaining desolventized wet meal C; specifically, the steam is ethanol steam, n-hexane steam and ethanol-n-hexane azeotropic steam.
Example 14
The embodiment provides a wet meal desolventizing method, which comprises the following steps:
freezing a cottonseed wet meal raw material at a temperature lower than zero degree, crushing the frozen cottonseed wet meal raw material into powder with the particle size of 150 meshes to obtain cottonseed meal particles, adding anhydrous ethanol with the weight of 23% of the weight of the cottonseed meal particles into the cottonseed meal particles, oscillating and dispersing the cottonseed meal particles, distilling the cottonseed meal particles at 67 ℃, adsorbing steam obtained by distillation by using the biochar-resin adsorbent D prepared in example 9, and obtaining desolventized wet meal D; specifically, the steam is ethanol steam, n-hexane steam and ethanol-n-hexane azeotropic steam.
Example 15
The embodiment provides a wet meal desolventizing method, which comprises the following steps:
freezing a cottonseed wet meal raw material at a temperature lower than zero degree, crushing the frozen cottonseed wet meal raw material into powder with the particle size of 50 meshes to obtain cottonseed meal particles, adding 27% by weight of absolute ethyl alcohol into the cottonseed meal particles, oscillating and dispersing the absolute ethyl alcohol, distilling the mixture at 80 ℃, adsorbing steam obtained by distillation by using the biochar-resin adsorbent E prepared in the embodiment 10, and obtaining desolventized wet meal E; specifically, the steam is ethanol steam, n-hexane steam and ethanol-n-hexane azeotropic steam.
Comparative example 1
The only difference between the specific method and the specific method in example 6 is that the weight parts of water, biochar, epoxy resin, polystyrene and binder are 13:60:15:5:6, preparing the cottonseed hull biochar a.
Comparative example 2
The only difference between the specific method and the example 7 is that the weight part ratio of water, biochar, epoxy resin, polystyrene and binder is 13:70:5:5:6, preparing the peanut shell biochar a.
Comparative example 3
The only difference between the specific method and the embodiment 8 is that the weight parts of water, biochar, epoxy resin, polystyrene and a binder are 13:80:13:5:6, preparing the cottonseed hull-peanut hull biochar a.
Comparative example 4
This comparative example provides a wet meal desolventizing method, which is the same as example 11, except that the specific adsorbent used the cottonseed hull biochar a prepared in comparative example 1.
Comparative example 5
The comparison example provides a wet meal desolventizing method, which is the same as that in example 11, and the only difference is that the peanut shell biochar a prepared in comparison example 1 is used as a specific adsorbent.
Comparative example 6
This comparative example provides a wet meal desolventizing method, which is the same as example 11, except that the specific adsorbent used the cottonseed hull-peanut hull biochar a prepared in comparative example 1.
Comparative example 7
This comparative example provides a wet meal desolventizing process, which is the same as example 11 except that the distillation temperature is 64 ℃.
Comparative example 8
This comparative example provides a wet meal desolventizing process, which is the same as example 11 except that the distillation temperature is 85 ℃.
Test example 1
The desolventizing wet meals A-E of examples 11-15 and comparative examples 4-8 are subjected to detection of n-hexane content and gossypol content, the method for determining the solvent residue is referred to GB 5009.262-2016, and the method for determining the gossypol content is referred to GB/T13086-2020. The measurement results are shown in table 1.
TABLE 1
| Free gossypol (mg/Kg) | N-hexane (mg/Kg) | |
| Maximum allowable amount | 60 | 10 |
| Example 11 | 42 | Undetected |
| Example 12 | 38 | Not detected out |
| Example 13 | 41 | Not detected out |
| Example 14 | 39 | Not detected out |
| Example 15 | 42 | Not detected out |
| Comparative example 4 | 54 | 8 |
| Comparative example 5 | 54 | Not detected out |
| Comparative example 6 | 52 | 9 |
| Comparative example 7 | 51 | 31 |
| Comparative example 8 | 43 | Not detected out |
From the test results, it can be seen that the desolventizing wet meal obtained in the embodiments 11 to 15 of the present invention is subjected to detection of the content of free gossypol and n-hexane, and n-hexane cannot be detected, and meanwhile, the content of free gossypol in the desolventizing wet meal is lower than the standard required by the industry, so that the n-hexane solvent and free gossypol can be effectively removed by using the wet meal desolventizing method disclosed by the present invention. The desolventized wet meal free gossypol obtained in comparative examples 4-8 can reach the standard, the n-hexane content in comparative examples 4, 5 and 6 can reach the industrial standard, but the effects of comparative examples 4, 5 and 6 are inferior to those of examples 11-15, namely the adsorbent in comparative examples 1-3; the n-hexane content of comparative example 7 was high because the distillation temperature was too low to completely distill n-hexane into vapor for adsorption. (ii) a Comparative example 8 the content of free gossypol and n-hexane in desolventized wet meal can reach the industrial standard, but the crude protein in the cottonseed meal is damaged due to overhigh distillation temperature, so that the nutritional value of the cottonseed meal is reduced.
In summary, the invention provides a wet meal desolventizing method, which comprises the steps of adding absolute ethyl alcohol into wet meal raw materials, vibrating and dispersing the absolute ethyl alcohol, distilling the wet meal raw materials, and adsorbing steam obtained by distillation by using a charcoal-resin adsorbent to obtain desolventized wet meal; specifically, the biochar-resin adsorbent consists of water, biochar, epoxy resin, polystyrene and a binder, wherein the biochar is cottonseed hulls and/or peanut hulls; by utilizing the wet meal desolventizing method disclosed by the invention, the n-hexane solvent and free gossypol can be effectively removed, so that the desolventized cottonseed meal meets the national standard; meanwhile, the wet meal raw material is treated by the ethanol, so that the wet meal can be effectively disinfected and sterilized, and the wet meal obtained by desolventizing can be directly used for preparing animal feed.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, many modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (9)
1. A wet meal desolventizing method is characterized by comprising the following steps:
adding absolute ethyl alcohol into wet meal raw materials, distilling after shaking and dispersing, and adsorbing steam obtained by distillation by using an adsorbent to obtain desolventized wet meal;
wherein the adsorbent is a biochar-resin adsorbent.
2. The wet meal desolventizing method according to claim 1, further comprising the following steps before adding the absolute ethyl alcohol: freezing and crushing the wet meal raw material to obtain cottonseed meal particles.
3. The wet meal desolventizing method according to claim 2, wherein the cottonseed meal particles have a particle size of 50-200 mesh.
4. The wet meal desolventizing method according to claim 1, wherein the temperature of the distillation is 67-80 ℃.
5. The wet meal desolventizing method according to claim 1, wherein the preparation method of the biochar-resin adsorbent is as follows:
uniformly mixing water, biochar, epoxy resin, polystyrene and a binder, plasticizing for 2-4h under a vacuum condition, and drying to obtain the biochar-resin adsorbent.
6. The wet meal desolventizing method according to claim 5, wherein the weight part ratio of the water, the biochar, the epoxy resin, the polystyrene and the binder is 9-13:65-70:8-15:3-5:3-6.
7. the wet meal desolventizing method according to claim 5, wherein the preparation method of the biochar is as follows:
crushing plant-based raw materials into powder with the particle size of 100-200 meshes, and then cracking at high temperature, wherein the cracking conditions are as follows: raising the temperature from room temperature to 500-600 ℃ at a constant speed at a speed of 8-12 ℃/min, keeping the temperature for 2-4h, and introducing CO 2 Activating for 0.5-1h, and then cooling to room temperature at a constant speed of 16-20 ℃/min to obtain the biochar.
8. The wet meal desolventizing method according to claim 7, wherein the plant-based raw material is cottonseed hulls and/or peanut hulls.
9. The wet meal desolventizing method according to claim 1, wherein the steam is ethanol steam, n-hexane steam and/or ethanol-n-hexane azeotropic steam.
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