CN114426474A - Preparation method of cottonseed oil and saponin biological stearic acid - Google Patents
Preparation method of cottonseed oil and saponin biological stearic acid Download PDFInfo
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- CN114426474A CN114426474A CN202111408735.4A CN202111408735A CN114426474A CN 114426474 A CN114426474 A CN 114426474A CN 202111408735 A CN202111408735 A CN 202111408735A CN 114426474 A CN114426474 A CN 114426474A
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- stearic acid
- cottonseed oil
- saponin
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- 235000012343 cottonseed oil Nutrition 0.000 title claims abstract description 51
- 235000021355 Stearic acid Nutrition 0.000 title claims abstract description 49
- 239000002385 cottonseed oil Substances 0.000 title claims abstract description 49
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 title claims abstract description 49
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000008117 stearic acid Substances 0.000 title claims abstract description 49
- 239000001397 quillaja saponaria molina bark Substances 0.000 title claims abstract description 39
- 229930182490 saponin Natural products 0.000 title claims abstract description 39
- 150000007949 saponins Chemical class 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims description 15
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 36
- 239000003921 oil Substances 0.000 claims abstract description 30
- 235000019198 oils Nutrition 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000007062 hydrolysis Effects 0.000 claims abstract description 18
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000007935 neutral effect Effects 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 37
- 239000003054 catalyst Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000007710 freezing Methods 0.000 claims description 14
- 230000008014 freezing Effects 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000010865 sewage Substances 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical group C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 14
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 10
- 235000014113 dietary fatty acids Nutrition 0.000 description 5
- 239000000194 fatty acid Substances 0.000 description 5
- 229930195729 fatty acid Natural products 0.000 description 5
- 238000007670 refining Methods 0.000 description 5
- 239000000344 soap Substances 0.000 description 5
- 239000013049 sediment Substances 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- -1 fatty acid sodium salt Chemical class 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- MCSXGCZMEPXKIW-UHFFFAOYSA-N 3-hydroxy-4-[(4-methyl-2-nitrophenyl)diazenyl]-N-(3-nitrophenyl)naphthalene-2-carboxamide Chemical group Cc1ccc(N=Nc2c(O)c(cc3ccccc23)C(=O)Nc2cccc(c2)[N+]([O-])=O)c(c1)[N+]([O-])=O MCSXGCZMEPXKIW-UHFFFAOYSA-N 0.000 description 1
- 235000019737 Animal fat Nutrition 0.000 description 1
- 206010003495 Aspermia Diseases 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000009874 alkali refining Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- FMMOOAYVCKXGMF-MURFETPASA-N ethyl linoleate Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(=O)OCC FMMOOAYVCKXGMF-MURFETPASA-N 0.000 description 1
- 229940031016 ethyl linoleate Drugs 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 208000000509 infertility Diseases 0.000 description 1
- 230000036512 infertility Effects 0.000 description 1
- 231100000535 infertility Toxicity 0.000 description 1
- 235000021190 leftovers Nutrition 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- FMMOOAYVCKXGMF-UHFFFAOYSA-N linoleic acid ethyl ester Natural products CCCCCC=CCC=CCCCCCCCC(=O)OCC FMMOOAYVCKXGMF-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000000920 spermatogeneic effect Effects 0.000 description 1
- 230000009261 transgenic effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/36—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by hydrogenation of carbon-to-carbon unsaturated bonds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
Abstract
The invention relates to the technical field of stearic acid processing, in particular to a method for preparing biological stearic acid by cottonseed oil and saponin, which sequentially comprises the steps of neutral oil separation, water washing, hydrolysis, hydrogenation and crystallization separation; according to the method for preparing the biological stearic acid from the cottonseed oil saponin, the biological stearic acid is prepared by recycling the cottonseed oil saponin, so that the recovery rate of stearic acid in the cottonseed oil saponin can be effectively improved.
Description
Technical Field
The invention relates to the technical field of stearic acid processing, and particularly relates to a preparation method of biological stearic acid with cottonseed oil and saponin.
Background
Cotton is an important fiber raw material and is one of five oil crops in China. The cottonseed oil is oil extracted from cottonseed, and is divided into pressed cottonseed oil, leached cottonseed oil, transgenic cottonseed oil, crude oil of cottonseed, and finished product cottonseed oil. The color is deep red compared with other oils, and the refined oil is edible for human, contains a large amount of fatty acids necessary for human body, and is most suitable for being mixed with animal fat for eating. However, the consumption of crude cottonseed oil can cause the damage of spermatogenic cells, resulting in aspermia and infertility. Cottonseed oil and saponin are the leftovers of the alkali refining and deacidification process of crude cotton oil, commonly called as 'cotton oil foot', are brown to dark brown black in color, and can become black and have foul smell after being stored in the air for a long time. The main components of the soap comprise neutral oil, soap and water, and also contain a small amount of protein, saccharide and unsaponifiable matter.
The components of the cottonseed oil saponin which are really available are neutral oil and fatty acid sodium salt, and the sum of the neutral oil and the fatty acid sodium salt accounts for 30-50% of the total saponin. At present, the soap is mainly utilized through two ways at home and abroad, firstly, the saponifiable matter is supplemented and saponified to prepare a soap base which is used as a raw material for preparing a series of washing products; secondly, the cottonseed oil saponin is firstly decomposed into fatty acid, then the fatty acid and the stearic acid are obtained by distillation, and then the oleic acid and the stearic acid are processed into industrial products, such as metal soap, barium stearate (zinc, aluminum, magnesium, cadmium) and the like, and can also be prepared into linoleic acid (pills), ethyl linoleate, floating agent and the like. The residue left after the oleic acid and the stearic acid are obtained by distillation can be processed into foundry sand adhesive, building waterproof material and the like. Because cottonseed oil saponin has wide sources and low price, the preparation cost of stearic acid can be greatly reduced by using the cottonseed oil saponin to prepare the stearic acid, but the recovery rate of stearic acid prepared by processing the cottonseed oil saponin in the prior art is lower, and the preparation process needs to be further improved.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for preparing biological stearic acid from cottonseed oil saponin, which can effectively improve the recovery rate of stearic acid in the cottonseed oil saponin by recycling the cottonseed oil saponin to prepare the biological stearic acid.
In order to achieve the technical effect, the invention adopts the following technical scheme:
a preparation method of biological stearic acid containing cottonseed oil and saponin comprises the following steps:
s1: separating neutral oil: placing cottonseed oil saponin into a reaction kettle, heating, adding a demulsifier, reacting under stirring, separating upper layer floating oil after reaction, and filtering a lower layer precipitate;
s2: washing with water: placing the lower-layer precipitate into a reaction kettle, adding pure water according to the material-liquid ratio of 10-15%, stirring for reaction, standing and separating sewage;
s3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 50-70 ℃, reacting for 2-5h, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid;
s4: hydrogenation: adding the hydrolyzed feed liquid into a hydrogenation kettle, adding a hydrogenation catalyst, reacting and hydrogenating, separating the hydrogenation catalyst after the reaction is finished, and reserving the feed liquid;
s5: and (3) crystallization separation: and (4) freezing and crystallizing the hydrogenated feed liquid.
Further, the demulsifier is sodium chloride.
Further, the hydrogenation catalyst is a palladium carbon catalyst or a raney nickel catalyst.
Further, the filtering method in the step S1 is filter pressing.
Further, the freezing temperature in the step S6 is-10 ℃ to-5 ℃.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a preparation method of biological stearic acid by cottonseed oil and saponin, which sequentially comprises the following steps: separating neutral oil, washing, hydrolyzing, hydrogenating, crystallizing and separating; the cottonseed oil saponin biological stearic acid preparation method recycles the cottonseed oil saponin to prepare the biological stearic acid, the treatment and preparation method is simple, the recovery rate of stearic acid in the existing cottonseed oil saponin can be effectively improved, and the prepared biological stearic acid meets the industrial standard
Detailed Description
The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby. The raw materials used in the examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art, unless otherwise specified.
Example 1
The embodiment provides a preparation method of biological stearic acid with cottonseed oil and saponin, which specifically comprises the following steps:
s1: separating neutral oil: 100kg of cottonseed oil saponin is placed in a reaction kettle, the temperature is raised to 40-60 ℃, 0.8 time of water by mass is added, 2% of sodium chloride is added to serve as a demulsifier, the reaction is carried out at constant temperature under the condition of stirring, the upper layer of floating oil is separated out through filter pressing after the reaction, the lower layer of sediment is left and filtered, and the upper layer of floating oil can be recycled and further used for cottonseed oil refining.
S2: washing with water: and (4) placing the lower-layer precipitate obtained in the step (S1) into a reaction kettle, adding pure water according to the material-liquid ratio of 10%, stirring for reaction for 1-2h, standing and separating sewage.
S3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 70 ℃, reacting for 2-5h for hydrolysis, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid;
s4: hydrogenation: and (4) adding the material liquid obtained after hydrolysis in the step (S3) into a hydrogenation kettle, adding a palladium-carbon catalyst as a hydrogenation catalyst, reacting for 5-6h at 180 ℃ under 1.5-2MPa, filtering and separating the hydrogenation catalyst after the reaction is finished, and reserving the material liquid.
S5: crystallization and separation: and (4) freezing and crystallizing the feed liquid subjected to the hydrogenation reaction in the step S5, wherein the freezing temperature is-5 ℃, so as to obtain the biological stearic acid.
The biological stearic acid prepared by the method meets the industrial standard, the recovery rate of stearic acid is about 76.3 percent, and the recovery rate is higher.
Example 2
The embodiment provides a preparation method of biological stearic acid with cottonseed oil and saponin, which specifically comprises the following steps:
s1: separating neutral oil: 100kg of cottonseed oil saponin is placed in a reaction kettle, the temperature is raised to 40-60 ℃, 0.6 time of water by mass is added, 1.8% of sodium chloride is added as a demulsifier, the reaction is carried out at constant temperature under the condition of stirring, the upper layer of floating oil is separated by filter pressing after the reaction, the lower layer of sediment is left and filtered, and the upper layer of floating oil can be recovered and further used for refining the cottonseed oil.
S2: washing with water: and (4) placing the lower-layer precipitate obtained in the step (S1) into a reaction kettle, adding pure water according to the feed-liquid ratio of 12%, stirring for reaction for 1-2h, standing and separating sewage.
S3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 50 ℃, reacting for 2-5h for hydrolysis, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid;
s4: hydrogenation: and (4) adding the material liquid obtained after hydrolysis in the step (S3) into a hydrogenation kettle, adding a palladium-carbon catalyst as a hydrogenation catalyst, reacting for 5-6h at 160 ℃ and 2MPa, filtering and separating the hydrogenation catalyst after the reaction is finished, and reserving the material liquid.
S5: and (3) crystallization separation: and (4) freezing and crystallizing the feed liquid subjected to the hydrogenation reaction in the step S5, wherein the freezing temperature is-5 ℃, so as to obtain the biological stearic acid.
The biological stearic acid prepared by the method meets the industrial standard, the recovery rate of stearic acid is about 78.8 percent, and the recovery rate is higher.
Example 3
The embodiment provides a preparation method of biological stearic acid with cottonseed oil and saponin, which specifically comprises the following steps:
s1: separating neutral oil: putting 120kg of cottonseed oil saponin into a reaction kettle, heating to 50-60 ℃, adding water according to the ratio of 1:1, adding 1.5% of sodium chloride as a demulsifier, reacting for 1-2h at constant temperature under stirring, separating upper-layer floating oil through pressure filtration after reaction, and reserving lower-layer precipitate for filtering, wherein the upper-layer floating oil can be recovered for further refining the cottonseed oil.
S2: washing with water: and (4) placing the lower-layer precipitate obtained in the step (S1) into a reaction kettle, adding pure water according to the feed-liquid ratio of 15%, stirring for reaction for 1-2h, standing and separating sewage.
S3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 60 ℃, reacting for 2-5h for hydrolysis, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid;
s4: hydrogenation: and (4) adding the material liquid obtained after hydrolysis in the step (S3) into a hydrogenation kettle, adding a palladium-carbon catalyst as a hydrogenation catalyst, reacting for 5-6h at 150 ℃ under 1.9MPa, filtering and separating the hydrogenation catalyst after the reaction is finished, and reserving the material liquid.
S5: and (3) crystallization separation: and (4) freezing and crystallizing the feed liquid subjected to the hydrogenation reaction in the step S5, wherein the freezing temperature is-5 ℃, so as to obtain the biological stearic acid.
The biological stearic acid prepared by the method meets the industrial standard, the recovery rate of stearic acid is about 74.2 percent, and the recovery rate is higher.
Example 4
The embodiment provides a preparation method of biological stearic acid with cottonseed oil and saponin, which specifically comprises the following steps:
s1: separating neutral oil: 100kg of cottonseed oil saponin is placed in a reaction kettle, the temperature is raised to 55 ℃, water is added according to the ratio of 1:1, 2% of sodium chloride is added as a demulsifier, the mixture reacts for 1.5 to 2 hours at constant temperature under the condition of stirring, the upper layer of floating oil is separated by pressure filtration after the reaction, the lower layer of sediment is left and filtered, and the upper layer of floating oil can be recovered and further used for refining the cottonseed oil.
S2: washing with water: and (4) placing the lower-layer precipitate obtained in the step (S1) into a reaction kettle, adding pure water according to the material-liquid ratio of 13%, stirring for reaction for 1-2h, standing and separating sewage.
S3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 60 ℃, reacting for 2-5h for hydrolysis, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid;
s4: hydrogenation: and (4) adding the feed liquid obtained after hydrolysis in the step S3 into a hydrogenation kettle, adding a palladium-carbon catalyst as a hydrogenation catalyst, reacting for 5 hours at 180 ℃ and under 2.2MPa, filtering and separating the hydrogenation catalyst after the reaction is finished, and reserving the feed liquid.
S5: and (3) crystallization separation: and (4) freezing and crystallizing the feed liquid subjected to the hydrogenation reaction in the step S5, wherein the freezing temperature is-5 ℃, so as to obtain the biological stearic acid.
The biological stearic acid prepared by the method meets the industrial standard, the recovery rate of the stearic acid is about 79.7 percent, and the recovery rate is higher.
Example 5
The embodiment provides a preparation method of biological stearic acid with cottonseed oil and saponin, which specifically comprises the following steps:
s1: separating neutral oil: 120kg of cottonseed oil saponin is placed in a reaction kettle, the temperature is raised to 60 ℃, water accounting for 60 percent of the mass of the materials is added, simultaneously, 2.5 percent of sodium chloride is added as a demulsifier, the mixture reacts for 1 hour under the condition of stirring at constant temperature, the upper layer of floating oil is separated out through filter pressing after the reaction, the lower layer of sediment is left and filtered, and the upper layer of floating oil can be recycled and further used for refining the cottonseed oil.
S2: washing with water: and (4) placing the lower-layer precipitate obtained in the step (S1) into a reaction kettle, adding pure water according to the material-liquid ratio of 10%, stirring for reaction for 1-2h, standing, separating sewage, and continuously washing twice.
S3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 60 ℃, reacting for 2-5h for hydrolysis, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid.
S4: hydrogenation: and (4) adding the material liquid obtained after hydrolysis in the step (S3) into a hydrogenation kettle, adding Raney nickel catalyst as a hydrogenation catalyst, reacting for 5 hours at 180 ℃ under 2.6MPa, filtering and separating the hydrogenation catalyst after the reaction is finished, and reserving the material liquid.
S5: and (3) crystallization separation: and (4) freezing and crystallizing the feed liquid subjected to the hydrogenation reaction in the step S5, wherein the freezing temperature is-10 ℃, so as to obtain the biological stearic acid.
The biological stearic acid prepared by the method meets the industrial standard, the recovery rate of stearic acid is about 78 and 6 percent, and the recovery rate is higher.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (5)
1. The preparation method of biological stearic acid from cottonseed oil and saponin is characterized by comprising the following steps:
s1: separating neutral oil: placing cottonseed oil saponin into a reaction kettle, heating, adding a demulsifier, reacting under stirring, separating upper layer floating oil after reaction, and filtering a lower layer precipitate;
s2: washing with water: placing the lower-layer precipitate into a reaction kettle, adding pure water according to the material-liquid ratio of 10-15%, stirring for reaction, standing and separating sewage;
s3: hydrolysis: adding sodium hydroxide aqueous solution into the washed feed liquid to adjust the pH value to 10-11, heating to 50-70 ℃, reacting for 2-5h, cooling, adding dilute sulfuric acid to adjust the pH value to 3-4, and separating out a water phase and the feed liquid;
s4: hydrogenation: adding the hydrolyzed feed liquid into a hydrogenation kettle, adding a hydrogenation catalyst, reacting and hydrogenating, separating the hydrogenation catalyst after the reaction is finished, and reserving the feed liquid;
s5: and (3) crystallization separation: and (4) freezing and crystallizing the hydrogenated feed liquid.
2. The method for preparing biological stearic acid from cottonseed oil saponin as claimed in claim 1, wherein: the demulsifier is sodium chloride.
3. The method for preparing biological stearic acid from cottonseed oil saponin as claimed in claim 1, wherein: the hydrogenation catalyst is a palladium carbon catalyst or a Raney nickel catalyst.
4. The method for preparing biological stearic acid from cottonseed oil saponin as claimed in claim 1, wherein: the filtering method in the step S1 is filter pressing.
5. The method for preparing biological stearic acid from cottonseed oil saponin as claimed in claim 1, wherein: the freezing temperature in the step S6 is-10 ℃ to-5 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101358160A (en) * | 2007-07-30 | 2009-02-04 | 孙树江 | Separation method of fat and soap stock at normal-temperature |
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