CN114989010A - Improved process for producing industrial oleic acid - Google Patents
Improved process for producing industrial oleic acid Download PDFInfo
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- CN114989010A CN114989010A CN202210803863.7A CN202210803863A CN114989010A CN 114989010 A CN114989010 A CN 114989010A CN 202210803863 A CN202210803863 A CN 202210803863A CN 114989010 A CN114989010 A CN 114989010A
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 title claims abstract description 56
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000005642 Oleic acid Substances 0.000 title claims abstract description 56
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 title claims abstract description 56
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 claims abstract description 30
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims abstract description 21
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims abstract description 21
- 238000001704 evaporation Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003463 adsorbent Substances 0.000 claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 76
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 239000013078 crystal Substances 0.000 claims description 27
- 238000003851 corona treatment Methods 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 18
- 239000011812 mixed powder Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- 239000005543 nano-size silicon particle Substances 0.000 claims description 17
- 235000012239 silicon dioxide Nutrition 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 16
- 239000011324 bead Substances 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 230000008020 evaporation Effects 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000199 molecular distillation Methods 0.000 claims description 9
- 238000007670 refining Methods 0.000 claims description 9
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 7
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000002689 soil Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 238000010296 bead milling Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 150000004671 saturated fatty acids Chemical class 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 150000002888 oleic acid derivatives Chemical class 0.000 description 1
- -1 polyene fatty acid Chemical class 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3021—Milling, crushing or grinding
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- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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Abstract
The invention discloses an improved process for producing industrial oleic acid, which belongs to the technical field of industrial oleic acid processing and comprises the following steps: s1, crystallizing and filter pressing; s2, adsorption treatment; s3, evaporating in a water bath; s4, rectification. The method improves the existing industrial oleic acid production process to a great extent, particularly separates saturated fatty acid and unsaturated fatty acid after crystallization and filter pressing, and then uses a special adsorbent for adsorption treatment, thereby obtaining high-purity oleic acid.
Description
Technical Field
The invention belongs to the technical field of industrial oleic acid processing, and particularly relates to an improved process for producing industrial oleic acid.
Background
Oleic acid (Oleieacid) is an important natural chemical substance and is one of the major fatty acids in lipoidal plants in organisms. As a fine chemical product, oleic acid and its derivatives have wide application. Particularly, with the development of new technologies such as modern biology, molecular biology, biophysics and the like, people are more and more aware of the very close relationship between oleic acid and life phenomena. Oleic acid is a necessary nutrient substance for human body, and plays a positive role in preventing and treating tumor particularly because the structure of the oleic acid is similar to that of polyene fatty acid such as linoleic acid, linolenic acid and the like, so that the oleic acid is difficult to separate from the fatty acid; and because the high-purity oleic acid has poor thermal stability and is interfered by various factors in the purification and separation processes, the high-purity oleic acid is difficult to obtain. Generally, the purity of the commercially available oleic acid is not high, the content of the oleic acid is less than 80%, and the color, smell, stability and safety of the commercially available oleic acid are not ideal. Thus limiting the application. The high-purity oleic acid hardly contains trace impurities such as oxides and the like, has good stability, no stimulation to skin and high safety, has excellent physical and chemical properties, and can be processed into high-purity oleic acid derivatives, so that the high-purity oleic acid is more suitable for application in the fields of medicines, cosmetics, bioengineering and the like, and therefore, the development and research of a preparation method of the high-purity high-yield oleic acid are very significant.
Disclosure of Invention
The invention aims to provide an improved process for producing industrial oleic acid aiming at the existing problems.
The invention is realized by the following technical scheme:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
adding natural oleic acid into acetone, mixing, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-20 to-15 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting acetone for later use;
s2, adsorption treatment:
adding an adsorbent into the acetone obtained in the step S1, then performing adsorption treatment in a constant-temperature ultrasonic environment, filtering after the adsorption treatment is completed, and collecting filtrate for later use;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Further, the weight volume ratio of the natural oleic acid to the acetone in the step S1 is 1g: 5-7 mL.
Further, the preparation of the adsorbent described in step S2 includes the following steps:
(1) bead grinding treatment:
putting montmorillonite soil and activated carbon together in a bead mill according to a weight ratio of 1: 4-6 for grinding to obtain mixed powder for later use;
(2) corona treatment:
placing the mixed powder obtained in the step (1) in a corona discharge instrument for corona treatment, and taking out for later use after the corona treatment is finished;
(3) flame treatment:
placing the nano silicon dioxide on flame outer flame for flame treatment, and taking out for later use after the flame treatment is finished;
(4) laser spraying treatment:
and (3) coating the flame-treated nano silicon dioxide on the surface of the corona-treated mixed powder by using a fluidized bed, and then carrying out ultraviolet irradiation treatment.
Further, the bead milling treatment in the step (1) is performed at a milling speed of 1000-2000 rpm for 30-50 min.
Further, the working voltage is controlled to be 10-14 kV during the corona treatment in the step (2), and the corona treatment time is 1-2 min.
Further, the horizontal distance between the nano silicon dioxide and the flame outer flame during the flame treatment in the step (3) is 30-50 mm, and the flame treatment time is 10-20 min.
Further, the constant temperature ultrasonic environment in step S2 is: the temperature is 60-80 ℃, and the ultrasonic frequency is 80-100 kHz.
Furthermore, the time of the adsorption treatment in the step S2 is 1-2 h.
Compared with the prior art, the invention has the following advantages:
the method improves the current industrial oleic acid production process to a great extent, particularly separates saturated fatty acid and unsaturated fatty acid after crystallization and filter pressing, and then uses a special adsorbent for adsorption treatment, thereby obtaining high-purity oleic acid.
Detailed Description
Example 1:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:5mL, stirring while carrying out programmed cooling, stopping stirring after white crystals are separated out, continuously cooling to-20 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting the acetone for later use;
s2, adsorption treatment:
adding an adsorbent into the acetone obtained in S1, then performing adsorption treatment in a constant-temperature ultrasonic environment at 60 ℃, wherein the ultrasonic frequency is 80kHz, filtering after 1h of adsorption treatment, and collecting filtrate for later use;
the preparation of the adsorbent comprises the following steps:
(1) bead grinding treatment:
putting montmorillonite soil and active carbon together in a bead mill according to a weight ratio of 1:4 for grinding, controlling the grinding speed to be 1000rpm, and performing bead milling for 30min to obtain mixed powder for later use;
(2) corona treatment:
placing the mixed powder obtained in the step (1) in a corona discharge instrument for corona treatment, controlling the working voltage to be 10kV, and taking out for later use after 1min of corona treatment;
(3) flame treatment:
placing the nano silicon dioxide on the flame outer flame for flame treatment, wherein the horizontal distance between the nano silicon dioxide and the flame outer flame is 30mm, and taking out for later use after flame treatment for 10 min;
(4) laser spray coating treatment:
coating the flame-treated nano silicon dioxide on the surface of the corona-treated mixed powder by using a fluidized bed, and then carrying out ultraviolet irradiation treatment;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Example 2:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:6mL, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-17.5 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting the acetone for later use;
s2, adsorption treatment:
adding an adsorbent into the acetone obtained in S1, then performing adsorption treatment in a constant-temperature ultrasonic environment at 70 ℃, wherein the ultrasonic frequency is 90kHz, filtering after the adsorption treatment is performed for 1.5h, and collecting filtrate for later use;
the preparation of the adsorbent comprises the following steps:
(1) bead grinding treatment:
putting montmorillonite soil and active carbon together in a bead mill according to a weight ratio of 1:5 for grinding, controlling the grinding speed to be 1500rpm, and performing bead mill treatment for 40min to obtain mixed powder for later use;
(2) corona treatment:
placing the mixed powder obtained in the step (1) in a corona discharge instrument for corona treatment, controlling the working voltage to be 12kV, and taking out for later use after 1.5min of corona treatment;
(3) flame treatment:
placing the nano silicon dioxide on the flame outer flame for flame treatment, wherein the horizontal distance between the nano silicon dioxide and the flame outer flame is 40mm, and taking out for later use after flame treatment for 15 min;
(4) laser spray coating treatment:
coating the flame-treated nano silicon dioxide on the surface of the corona-treated mixed powder by using a fluidized bed, and performing ultraviolet irradiation treatment after the coating is finished;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Example 3:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:7mL, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-15 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting the acetone for later use;
s2, adsorption treatment:
adding an adsorbent into the acetone obtained in S1, then performing adsorption treatment in a constant-temperature ultrasonic environment at 80 ℃, wherein the ultrasonic frequency is 100kHz, filtering after 2h of adsorption treatment, and collecting filtrate for later use;
the preparation of the adsorbent comprises the following steps:
(1) bead grinding treatment:
grinding montmorillonite soil and active carbon together in a bead mill at a weight ratio of 1:6 at a grinding speed of 2000rpm for 50min to obtain mixed powder;
(2) corona treatment:
placing the mixed powder obtained in the step (1) in a corona discharge instrument for corona treatment, controlling the working voltage to be 14kV, and taking out for later use after corona treatment for 2 min;
(3) flame treatment:
placing the nano silicon dioxide on flame outer flame for flame treatment, wherein the horizontal distance between the nano silicon dioxide and the flame outer flame is 50mm, and taking out for later use after flame treatment for 20 min;
(4) laser spraying treatment:
coating the flame-treated nano silicon dioxide on the surface of the corona-treated mixed powder by using a fluidized bed, and performing ultraviolet irradiation treatment after the coating is finished;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Comparative example 1:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:6mL, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-17.5 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting the acetone for later use;
s2, adsorption treatment:
adding montmorillonite into the acetone obtained in S1, performing adsorption treatment in a constant-temperature ultrasonic environment at 70 ℃, performing adsorption treatment for 1.5h at an ultrasonic frequency of 90kHz, filtering, and collecting filtrate for later use;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Comparative example 2:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:6mL, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-17.5 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting the acetone for later use;
s2, adsorption treatment:
adding activated carbon into the acetone obtained in S1, then performing adsorption treatment in a constant-temperature ultrasonic environment at 70 ℃, wherein the ultrasonic frequency is 90kHz, filtering after the adsorption treatment is performed for 1.5h, and collecting filtrate for later use;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Comparative example 3:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:6mL, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-17.5 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting the acetone for later use;
s2, adsorption treatment:
adding an adsorbent into the acetone obtained in the step S1, then performing adsorption treatment at a constant temperature of 70 ℃, filtering after the adsorption treatment for 1.5h, and collecting filtrate for later use;
the preparation of the adsorbent comprises the following steps:
(1) bead grinding treatment:
grinding montmorillonite soil and active carbon together in a bead mill according to a weight ratio of 1:5, controlling the grinding speed to be 1500rpm, and performing bead milling for 40min to obtain mixed powder for later use;
(2) corona treatment:
placing the mixed powder obtained in the step (1) in a corona discharge instrument for corona treatment, controlling the working voltage to be 12kV, and taking out for later use after 1.5min of corona treatment;
(3) flame treatment:
placing the nano silicon dioxide on the flame outer flame for flame treatment, wherein the horizontal distance between the nano silicon dioxide and the flame outer flame is 40mm, and taking out for later use after flame treatment for 15 min;
(4) laser spray coating treatment:
coating the flame-treated nano silicon dioxide on the surface of the corona-treated mixed powder by using a fluidized bed, and performing ultraviolet irradiation treatment after the coating is finished;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
Comparative example 4:
an improved process for producing industrial oleic acid comprises the following steps:
s1, crystallizing and pressure filtering:
mixing natural oleic acid and acetone according to the weight-volume ratio of 1g:6mL, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-17.5 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting acetone for later use;
s2, evaporating in water bath:
putting the acetone obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering the acetone;
s3, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S2 under the pressure of 133.3 MPa.
Control group:
the application numbers are: CN201810298614.0 discloses a production process and a device for industrial oleic acid.
In order to compare the technical effects of the application, the methods of example 2 and comparative examples 1-4 are respectively used for preparing oleic acid correspondingly, and then the yield and the purity are measured.
The specific experimental comparative data are shown in the following table 1:
TABLE 1
As can be seen from table 1 above, the present application is greatly improved in the present industrial oleic acid production process, and particularly, after crystallization and pressure filtration are performed, saturated fatty acid and unsaturated fatty acid are separated, and then a special adsorbent is used for adsorption treatment, so that high-purity oleic acid is obtained, which has great market popularization significance.
Claims (8)
1. An improved process for producing industrial oleic acid is characterized by comprising the following steps:
s1, crystallizing and pressure filtering:
adding natural oleic acid into acetone, mixing, carrying out programmed cooling while stirring, stopping stirring after white crystals are separated out, continuously cooling to-20 to-15 ℃, fully separating out the crystals, carrying out filter pressing after no new crystals are separated out, and collecting acetone for later use;
s2, adsorption treatment:
adding an adsorbent into the acetone obtained in the step S1, then performing adsorption treatment in a constant-temperature ultrasonic environment, filtering after the adsorption treatment is completed, and collecting filtrate for later use;
s3, evaporating in water bath:
putting the filtrate obtained in the step S2 on a water bath for evaporation to obtain unsaturated fatty acid for later use, and simultaneously recovering acetone;
s4, rectification:
and (4) performing molecular distillation refining on the unsaturated fatty acid obtained in the step S3 under the pressure of 133.3 MPa.
2. The improved process for producing industrial oleic acid according to claim 1, wherein the weight-to-volume ratio of the natural oleic acid and acetone in the step S1 is 1g: 5-7 mL.
3. The improved process for industrial production of oleic acid according to claim 1, wherein the preparation of the adsorbent in step S2 comprises the following steps:
(1) bead grinding treatment:
putting montmorillonite soil and activated carbon together in a bead mill according to a weight ratio of 1: 4-6 for grinding to obtain mixed powder for later use;
(2) corona treatment:
placing the mixed powder obtained in the step (1) in a corona discharge instrument for corona treatment, and taking out for later use after the corona treatment is finished;
(3) flame treatment:
placing the nano silicon dioxide on flame outer flame for flame treatment, and taking out for later use after the flame treatment is finished;
(4) laser spraying treatment:
and (3) coating the flame-treated nano silicon dioxide on the surface of the corona-treated mixed powder by using a fluidized bed, and then carrying out ultraviolet irradiation treatment.
4. The improved process for producing industrial oleic acid according to claim 3, characterized in that the bead milling treatment in the step (1) is carried out at a milling speed of 1000-2000 rpm for 30-50 min.
5. The improved process for producing industrial oleic acid according to claim 3, characterized in that the working voltage during the corona treatment in the step (2) is controlled to be 10-14 kV, and the time of the corona treatment is 1-2 min.
6. The improved process for producing industrial oleic acid according to claim 3, characterized in that the horizontal distance between the nano-silica and the flame outer flame during the flame treatment in the step (3) is 30-50 mm, and the flame treatment time is 10-20 min.
7. The improved process for producing industrial oleic acid according to claim 1, wherein the constant temperature ultrasonic environment in step S2 is: the temperature is 60-80 ℃, and the ultrasonic frequency is 80-100 kHz.
8. The improved process for producing industrial oleic acid according to claim 1, wherein the adsorption treatment time in the step S2 is 1-2 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0225946A1 (en) * | 1985-12-05 | 1987-06-24 | Nippon Oil And Fats Company, Limited | Method of producing oleic acid |
| CN108558644A (en) * | 2018-04-04 | 2018-09-21 | 赞宇科技集团股份有限公司 | A kind of production technology and device of industrial oleic acid |
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2022
- 2022-07-07 CN CN202210803863.7A patent/CN114989010A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0225946A1 (en) * | 1985-12-05 | 1987-06-24 | Nippon Oil And Fats Company, Limited | Method of producing oleic acid |
| CN108558644A (en) * | 2018-04-04 | 2018-09-21 | 赞宇科技集团股份有限公司 | A kind of production technology and device of industrial oleic acid |
Non-Patent Citations (2)
| Title |
|---|
| 杨继生等: "高纯油酸的性能、制备及应用", 上海化工, vol. 24, no. 18, pages 28 - 30 * |
| 郭霞等: "油酸的生产工艺及应用", 广州化工, vol. 45, no. 24, pages 6 - 8 * |
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