CN117247809A - Rectification process and production system of high-carbon fatty acid - Google Patents
Rectification process and production system of high-carbon fatty acid Download PDFInfo
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- CN117247809A CN117247809A CN202311358877.3A CN202311358877A CN117247809A CN 117247809 A CN117247809 A CN 117247809A CN 202311358877 A CN202311358877 A CN 202311358877A CN 117247809 A CN117247809 A CN 117247809A
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- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 119
- 239000000194 fatty acid Substances 0.000 title claims abstract description 119
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 119
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 60
- 238000000926 separation method Methods 0.000 claims abstract description 56
- 239000012535 impurity Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims abstract description 26
- 238000001179 sorption measurement Methods 0.000 claims abstract description 25
- 230000018044 dehydration Effects 0.000 claims abstract description 22
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 230000007062 hydrolysis Effects 0.000 claims abstract description 18
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims description 26
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 15
- 239000001506 calcium phosphate Substances 0.000 claims description 9
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 9
- 235000011010 calcium phosphates Nutrition 0.000 claims description 9
- 229920002301 cellulose acetate Polymers 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 235000013311 vegetables Nutrition 0.000 claims description 2
- 239000000047 product Substances 0.000 description 26
- 239000000203 mixture Substances 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000004519 grease Substances 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- -1 diglyceride Chemical compound 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000001261 hydroxy acids Chemical class 0.000 description 1
- 238000009776 industrial production Methods 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
- 239000007791 liquid phase Substances 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 150000004667 medium chain fatty acids Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000004666 short chain fatty acids Chemical class 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 150000005672 tetraenes Chemical class 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/04—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a rectification process and a production system of high-carbon fatty acid, and belongs to the technical field of high-carbon fatty acid. S1, conveying plant acidified oil and water to a pressurizing hydrolysis device, and introducing high-pressure steam to perform heating treatment to obtain crude fatty acid mixed solution; s2, feeding the crude fatty acid mixed solution into a separation and impurity removal device for separation and impurity removal treatment to obtain primary fatty acid; the separation and impurity removal treatment comprises oil-water separation, adsorption impurity removal and solid-liquid separation; s3, sending the primary fatty acid into a vacuum dehydration device for vacuum dehydration treatment to obtain medium-grade fatty acid; s4, sending the medium-grade fatty acid into a multi-stage rectifying device for multi-stage rectifying treatment to obtain high-carbon fatty acid; the multistage rectification treatment is divided into a primary rectification treatment, a secondary rectification treatment and a tertiary rectification treatment. The yield and purity of the high-carbon fatty acid are effectively improved by adding modified calcium phosphate and combining a multistage rectification process.
Description
Technical Field
The invention belongs to the technical field of high-carbon fatty acid, and particularly relates to a rectification process and a production system of high-carbon fatty acid.
Background
The acidified oil is an oil obtained by acidifying soapstock, a byproduct produced by a fat refinery, and is essentially fatty acid, and contains various components such as pigment, non-acidified triglyceride, diglyceride, monoglyceride (neutral oil), etc. Fatty acids are important basic materials for oil and fat chemical industry. The length of the carbon chain in the molecular structure of fatty acid is classified into three types of short chain fatty acid (less than 6 carbon atoms in the carbon chain), medium chain fatty acid (6-12 carbon atoms in the carbon chain) and long chain fatty acid (i.e. high carbon fatty acid, more than 12 carbon atoms in the carbon chain). Downstream derivatives produced by taking high-carbon fatty acid as raw materials are widely applied to the fields of medicine, daily chemical industry, rubber and plastic processing and the like. With the rapid development of the age, the consumption of high-carbon fatty acids is continuously increased, and the demand for high-carbon fatty acids is rapidly increased. Therefore, the research on the efficient and energy-saving preparation process of the high-carbon fatty acid has important practical significance.
The existing fatty acid production processes mainly comprise two types: firstly, normal pressure hydrolysis: adding grease and a catalyst into a reaction kettle, stirring and heating the mixture for reaction for 20 to 24 hours by a mode of directly entering steam, standing and layering the mixture to discharge glycerin at the bottom, then supplementing the catalyst and sulfuric acid aqueous solution again, and repeating the operation until the hydrolysis rate can reach 92 to 95 percent. The fatty acid has the characteristics and defects of intermittent operation, complex operation, long reaction time and low production efficiency. And secondly, high-pressure hydrolysis: the oil is added into the reaction kettle, and the solubility of the oil in water is increased under the action of high temperature and high pressure, so that the reaction rate can be increased, and the hydrolysis rate can be improved. The main technological parameters of the method are as follows: the operation temperature is 255-265 ℃, the operation pressure is 5.5-6.5 MPa, the reaction time is 1-3 h, the high-pressure hydrolysis method has the advantages that the hydrolysis rate can reach 98 percent, but the raw material cost is high, the reaction temperature is higher (the grease is easy to produce side reaction when the reaction temperature is more than 260 ℃), the energy consumption is increased, the applicability is affected by the requirement on the reaction raw material (the high-pressure hydrolysis technology is not suitable for the grease containing more linolenic acid, conjugated double bonds, hydroxy acid and tetraene, and the like), and the requirements of the industrial large-scale preparation of high-quality high-carbon fatty acid cannot be met by the methods.
The rectification method realizes separation and storage according to different carbon chain lengths and different boiling points of fatty acids. The traditional high-carbon fatty acid recovery device mostly adopts batch kettle type single-tower continuous rectification. The batch kettle type distillation process is simple, but has higher energy consumption, and the single-tower single-effect rectification process has lower energy consumption than the batch kettle type distillation process, but has poor product quality. The phenomenon that the traditional high-carbon fatty acid rectifying device wastes high-carbon fatty acid is serious in the rectifying process, and the high-carbon fatty acid carried in the noncondensable gas at the top of the rectifying tower can not be effectively recycled and reprocessed, so that huge waste can be caused in the production process.
In order to meet the requirements of high-purity high-carbon fatty acid in industrial production, development of a process method with high product yield and high purity of high-carbon fatty acid is needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides a rectification process and a production system of high-carbon fatty acid.
The first object of the present invention is to provide a process for producing high-carbon fatty acid, comprising the steps of,
s1, conveying plant acidified oil and water to a pressurizing hydrolysis device, and introducing high-pressure steam to perform heating treatment to obtain crude fatty acid mixed solution;
s2, sending the crude fatty acid mixed solution obtained in the step S1 into a separation and impurity removal device for separation and impurity removal treatment to obtain primary fatty acid;
the separation and impurity removal treatment comprises oil-water separation, adsorption impurity removal and solid-liquid separation;
s3, sending the primary fatty acid in the S2 into a vacuum dehydration device for vacuum dehydration treatment to obtain medium-grade fatty acid;
s4, sending the medium-grade fatty acid in the S3 into a multi-stage rectifying device for multi-stage rectifying treatment to obtain high-carbon fatty acid;
the multi-stage rectification treatment comprises a primary rectification treatment, a secondary rectification treatment and a tertiary rectification treatment, wherein the heavy component product which is not gasified in the primary rectification treatment is a raw material of the secondary rectification treatment, and the heavy component product which is not gasified in the secondary rectification treatment is a raw material of the tertiary rectification treatment; and cooling the gasified light component products in the primary rectification treatment, the secondary rectification treatment and the tertiary rectification treatment to obtain high-carbon fatty acid refined products.
In one embodiment of the present invention, in S1, the mass ratio of the vegetable acidified oil to water is 1:1-1.2.
In one embodiment of the present invention, in S1, the heating treatment is performed at a pressure of 3.5MPa to 4.0MPa, a temperature of 230 ℃ to 250 ℃ and a time of 7h to 8h.
In one embodiment of the present invention, in S2, the adsorption impurity removal is to add modified calcium phosphate to an oil layer obtained by oil-water separation for adsorption.
In one embodiment of the invention, the preparation method of the modified calcium phosphate comprises the following steps:
s21, dissolving 2-4 parts by mass of cellulose acetate in 100-120 parts by mass of acetone to obtain a cellulose acetate solution;
dissolving 20-24 parts by mass of calcium phosphate in 130-150 parts by mass of water to obtain a calcium phosphate suspension;
s22, dropwise adding the calcium phosphate suspension liquid obtained in the S21 into a cellulose acetate solution to obtain a mixed solution;
s23, adding the mixed solution obtained in the step S22 into water at the temperature of 40-45 ℃, stirring for 30-40 min, filtering, and drying under reduced pressure to obtain the modified calcium phosphate.
In one embodiment of the invention, the mass ratio of the oil layer to the modified calcium phosphate is 1:0.1-0.12.
In one embodiment of the present invention, in S3, the temperature of the vacuum dehydration treatment is 160 ℃ to 230 ℃; the vacuum degree is 90KPa-100KPa; the time is 5min-40min. The vacuum dehydration treatment not only can dehydrate, but also can degas, remove low-boiling substances, and further improve the purity of the high-carbon fatty acid.
In one embodiment of the invention, in S4, the reaction temperature of the primary rectification process is 350-380 ℃ and the vacuum degree is 2.5KPa-3.0KPa; the reaction temperature of the secondary rectification process is 340-350 ℃ and the vacuum degree is 2.0KPa-2.5KPa; the reaction temperature of the three-stage rectification process is 330-340 ℃ and the vacuum degree is 1.5KPa-2.0KPa.
The second object of the invention is to provide a high-carbon fatty acid production system, which comprises a pressurizing hydrolysis device, a separating and impurity removing device, a vacuum dehydration device and a multistage rectifying device which are sequentially arranged;
the separation impurity removing device comprises an oil-water separation device, an adsorption impurity removing device and a solid-liquid separation device which are sequentially arranged;
the multistage rectifying device comprises a primary rectifying device, a secondary rectifying device and a tertiary rectifying device which are sequentially arranged, wherein a heavy component material outlet of the primary rectifying device is communicated with a material inlet of the secondary rectifying device through a primary heavy component pipeline, and a heavy component material outlet of the secondary rectifying device is communicated with a material inlet of the tertiary rectifying device through a secondary heavy component pipeline.
In one embodiment of the invention, the primary rectification device comprises a primary rectification tower and a primary hydrazine cooler; the secondary rectifying device comprises a secondary rectifying tower and a secondary hydrazine cooler; the three-stage rectifying device comprises a three-stage rectifying tower and a three-stage hydrazine cooler.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) According to the production process of the high-carbon fatty acid, the modified calcium phosphate is added to selectively adsorb part of nitrogen-containing and sulfur-containing components in the high-carbon fatty acid, and impurities are removed in advance before rectification, so that the content of the high-carbon fatty acid impurities can be reduced. Meanwhile, the multi-stage rectification process is combined, so that the yield and purity of the high-carbon fatty acid are effectively improved.
(2) The production process of the high-carbon fatty acid adopts a multistage rectification process, takes medium-grade fatty acid as a raw material, and separates the medium-grade fatty acid into light components and heavy components by continuous feeding under the action of a high-vacuum rectification tower and utilizing the difference of boiling points of the materials, thereby finally obtaining a refined fatty acid product.
(3) The production systems of the high-carbon fatty acid are all conventional equipment in the field, and have low requirements on the equipment; avoiding the use of organic solvents, greatly saving the cost and reducing the environmental pollution.
Drawings
In order that the invention may be more readily understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings, in which:
FIG. 1 is a schematic diagram of a system for producing higher fatty acids according to the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
In the present invention, unless otherwise specified, the production system of high-carbon fatty acid is shown in fig. 1, comprising a pressurized hydrolysis device, a separation and impurity removal device, a vacuum dehydration device and a multistage rectification device which are arranged in this order; the separation impurity removing device comprises an oil-water separating device, an adsorption impurity removing device and a solid-liquid separating device which are sequentially arranged; the multistage rectifying device comprises a first-stage rectifying device, a second-stage rectifying device and a third-stage rectifying device which are sequentially arranged, wherein a heavy component material outlet of the first-stage rectifying device is communicated with a material inlet of the second-stage rectifying device through a first-stage heavy component pipeline, and a heavy component material outlet of the second-stage rectifying device is communicated with a material inlet of the third-stage rectifying device through a second-stage heavy component pipeline. Each level of rectifying device comprises a rectifying tower, a hydrazine cooler, a heavy component tank, a heavy component pump, a light component tank and a light component pump. Taking a primary rectifying device as an example: the feed inlet of the primary rectifying tower is connected with a feed pipeline, and the feed pipeline is used for driving the medium-grade fatty acid into the primary rectifying tower to carry out primary rectification. The light component outlet of the first-stage rectifying tower is communicated with the inlet of the first-stage hydrazine cooler, the outlet of the first-stage hydrazine cooler is communicated with the inlet of the first-stage light component tank, the outlet of the first-stage light component tank is communicated with a first-stage light component pipeline, and a first-stage light component pump is arranged on the first-stage light component pipeline. The heavy component outlet of the first-stage rectifying tower is communicated with the inlet of the first-stage heavy component tank, the outlet of the first-stage heavy component tank is communicated with the first-stage heavy component pipeline, the outlet of the first-stage heavy component tank is communicated with the feed inlet of the second-stage rectifying device through the first-stage heavy component pipeline, and the first-stage heavy component pipeline is provided with a first-stage heavy component pump. After the medium-grade fatty acid is pumped into the first-grade rectifying tower through a feeding pipeline, the light-component substances are changed from liquid phase into gas phase, enter the first-grade hydrazine cooler, become high-carbon fatty acid refined products after cooling, enter the first-grade light-component tank, and are pumped out through the first-grade light-component pump. The heavy component materials which are not gasified in the primary rectifying tower flow into the primary heavy component tank from the heavy component outlet of the primary rectifying tower, and are continuously pumped into the secondary rectifying device by the primary heavy component pump to carry out secondary rectification.
In the present invention, the preparation method of the modified calcium phosphate comprises the following steps, unless otherwise specified: dissolving 3 parts by mass of cellulose acetate in 110 parts by mass of acetone to obtain a cellulose acetate solution; dissolving 22 parts by mass of calcium phosphate in 140 parts by mass of water to obtain a calcium phosphate suspension; dropwise adding the calcium phosphate suspension into a cellulose acetate solution to obtain a mixed solution; adding the mixed solution into water at 42 ℃, stirring for 35min, filtering out the solidification, and drying under reduced pressure to obtain the modified calcium phosphate.
Example 1
The production process of the high-carbon fatty acid specifically comprises the following steps:
s1, plant acidified oil and water are mixed according to a mass ratio of 1:1.1, sending the mixture to a pressurized hydrolysis device, introducing high-pressure steam for heating treatment, setting the pressure of the heating treatment to be 3.8MPa, the temperature to be 240 ℃ and the time to be 7.5 hours, and obtaining crude fatty acid mixed solution;
s2, feeding the crude fatty acid mixed solution into a separation and impurity removal device (an oil-water separation device, an adsorption and impurity removal device and a solid-liquid separation device), and firstly performing oil-water separation in the oil-water separation device, wherein the obtained oil layer and modified calcium phosphate are prepared according to a mass ratio of 1:0.11, performing adsorption impurity removal in an adsorption impurity removal device, performing solid-liquid separation in a solid-liquid separation device after adsorption is completed, and discarding a solid phase to obtain primary fatty acid;
s3, feeding the primary fatty acid into a vacuum dehydration device for vacuum dehydration treatment, wherein the set temperature is 200 ℃; the vacuum degree is 95KPa; the time is 10min, and the medium-grade fatty acid is obtained;
s4, sending the medium-grade fatty acid into a multi-stage rectifying device (a first-stage rectifying device, a second-stage rectifying device and a third-stage rectifying device) for multi-stage rectifying treatment, wherein a heavy component product which is not gasified in the first-stage rectifying device enters the second-stage rectifying device, and a heavy component product which is not gasified in the second-stage rectifying device is the third-stage rectifying device; the gasified light component products in the primary rectifying device, the secondary rectifying device and the tertiary rectifying device are cooled to obtain high-carbon fatty acid refined products, the purity of the high-carbon fatty acid is 92.8%, and the yield is 63%;
wherein, the reaction temperature of the primary rectifying device is 375 ℃, and the vacuum degree is 2.8KPa;
the reaction temperature of the secondary rectifying device is 345 ℃, and the vacuum degree is 2.3KPa;
the reaction temperature of the three-stage rectifying device is 335 ℃, and the vacuum degree is 1.7KPa.
Example 2
The production process of the high-carbon fatty acid specifically comprises the following steps:
s1, plant acidified oil and water are mixed according to a mass ratio of 1:1.2, sending the mixture to a pressurized hydrolysis device, introducing high-pressure steam for heating treatment, setting the pressure of the heating treatment to be 4.0MPa, the temperature to be 250 ℃ and the time to be 7 hours, and obtaining crude fatty acid mixed solution;
s2, feeding the crude fatty acid mixed solution into a separation and impurity removal device (an oil-water separation device, an adsorption and impurity removal device and a solid-liquid separation device), and firstly performing oil-water separation in the oil-water separation device, wherein the obtained oil layer and modified calcium phosphate are prepared according to a mass ratio of 1:0.12, the mixture enters an adsorption impurity removal device for adsorption impurity removal, and after adsorption, the mixture enters a solid-liquid separation device for solid-liquid separation, and a solid phase is discarded to obtain primary fatty acid;
s3, feeding the primary fatty acid into a vacuum dehydration device for vacuum dehydration treatment, wherein the set temperature is 230 ℃; the vacuum degree is 100KPa; obtaining the medium-grade fatty acid after 5 min;
s4, sending the medium-grade fatty acid into a multi-stage rectifying device (a first-stage rectifying device, a second-stage rectifying device and a third-stage rectifying device) for multi-stage rectifying treatment, wherein a heavy component product which is not gasified in the first-stage rectifying device enters the second-stage rectifying device, and a heavy component product which is not gasified in the second-stage rectifying device is the third-stage rectifying device; the gasified light component products in the primary rectifying device, the secondary rectifying device and the tertiary rectifying device are cooled to obtain high-carbon fatty acid refined products, the purity of the high-carbon fatty acid is 89.4%, and the yield is 59%;
wherein the reaction temperature of the primary rectification is 380 ℃ and the vacuum degree is 2.5KPa;
the reaction temperature of the secondary rectification is 350 ℃ and the vacuum degree is 2.0KPa;
the reaction temperature of the three-stage rectification is 340 ℃ and the vacuum degree is 1.5KPa.
Example 3
The production process of the high-carbon fatty acid specifically comprises the following steps:
s1, plant acidified oil and water are mixed according to a mass ratio of 1:1, sending the mixture to a pressurized hydrolysis device, introducing high-pressure steam for heating treatment, setting the pressure of the heating treatment to be 3.5MPa, the temperature to be 230 ℃ and the time to be 8 hours, and obtaining crude fatty acid mixed solution;
s2, feeding the crude fatty acid mixed solution into a separation and impurity removal device (an oil-water separation device, an adsorption and impurity removal device and a solid-liquid separation device), and firstly performing oil-water separation in the oil-water separation device, wherein the obtained oil layer and modified calcium phosphate are prepared according to a mass ratio of 1:0.1, entering an adsorption impurity removal device for adsorption impurity removal, and after adsorption, entering a solid-liquid separation device for solid-liquid separation, and discarding a solid phase to obtain primary fatty acid;
s3, feeding the primary fatty acid into a vacuum dehydration device for vacuum dehydration treatment, wherein the set temperature is 160 ℃; the vacuum degree is 90KPa; the time is 40min, and the medium-grade fatty acid is obtained;
s4, sending the medium-grade fatty acid into a multi-stage rectifying device (a first-stage rectifying device, a second-stage rectifying device and a third-stage rectifying device) for multi-stage rectifying treatment, wherein a heavy component product which is not gasified in the first-stage rectifying device enters the second-stage rectifying device, and a heavy component product which is not gasified in the second-stage rectifying device is the third-stage rectifying device; the gasified light component products in the primary rectifying device, the secondary rectifying device and the tertiary rectifying device are cooled to obtain high-carbon fatty acid refined products; the purity of the high-carbon fatty acid is 90.3 percent, and the yield is 58 percent;
wherein, the reaction temperature of the primary rectification is 350 ℃ and the vacuum degree is 3.0KPa;
the reaction temperature of the secondary rectification is 340 ℃, and the vacuum degree is 2.5KPa;
the reaction temperature of the three-stage rectification is 330 ℃, and the vacuum degree is 2.0KPa.
Comparative example 1
Substantially the same as in example 1, except that modified calcium phosphate was not used:
s1, plant acidified oil and water are mixed according to a mass ratio of 1:1.1, sending the mixture to a pressurized hydrolysis device, introducing high-pressure steam for heating treatment, setting the pressure of the heating treatment to be 3.8MPa, the temperature to be 240 ℃ and the time to be 7.5 hours, and obtaining crude fatty acid mixed solution;
s2, feeding the crude fatty acid mixed solution into an oil-water separation device for oil-water separation to obtain primary fatty acid;
s3, feeding the primary fatty acid into a vacuum dehydration device for vacuum dehydration treatment, wherein the set temperature is 200 ℃; the vacuum degree is 95KPa; the time is 10min, and the medium-grade fatty acid is obtained;
s4, sending the medium-grade fatty acid into a multi-stage rectifying device (a first-stage rectifying device, a second-stage rectifying device and a third-stage rectifying device) for multi-stage rectifying treatment, wherein a heavy component product which is not gasified in the first-stage rectifying device enters the second-stage rectifying device, and a heavy component product which is not gasified in the second-stage rectifying device is the third-stage rectifying device; the gasified light component products in the primary rectifying device, the secondary rectifying device and the tertiary rectifying device are cooled to obtain high-carbon fatty acid refined products; the purity of the high-carbon fatty acid is 81.5 percent, and the yield is 60 percent;
wherein, the reaction temperature of the primary rectifying device is 375 ℃, and the vacuum degree is 2.8KPa;
the reaction temperature of the secondary rectifying device is 345 ℃, and the vacuum degree is 2.3KPa;
the reaction temperature of the three-stage rectifying device is 335 ℃, and the vacuum degree is 1.7KPa.
Comparative example 2
Substantially the same as in example 1, except that multistage rectification was not conducted:
s1, plant acidified oil and water are mixed according to a mass ratio of 1:1.1, sending the mixture to a pressurized hydrolysis device, introducing high-pressure steam for heating treatment, setting the pressure of the heating treatment to be 3.8MPa, the temperature to be 240 ℃ and the time to be 7.5 hours, and obtaining crude fatty acid mixed solution;
s2, feeding the crude fatty acid mixed solution into a separation and impurity removal device (an oil-water separation device, an adsorption and impurity removal device and a solid-liquid separation device), and firstly performing oil-water separation in the oil-water separation device, wherein the obtained oil layer and modified calcium phosphate are prepared according to a mass ratio of 1:0.11, performing adsorption impurity removal in an adsorption impurity removal device, performing solid-liquid separation in a solid-liquid separation device after adsorption is completed, and discarding a solid phase to obtain primary fatty acid;
s3, feeding the primary fatty acid into a vacuum dehydration device for vacuum dehydration treatment, wherein the set temperature is 200 ℃; the vacuum degree is 95KPa; the time is 10min, and the medium-grade fatty acid is obtained;
s4, sending the medium-grade fatty acid into a rectifying device, setting the reaction temperature of the rectifying device to 375 ℃, and the vacuum degree to 2.8KPa, wherein the gasified light component product in the rectifying device is the high-carbon fatty acid refined product after being cooled; the purity of the high-carbon fatty acid was 77.2%, and the yield was 47%.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (9)
1. A process for preparing high-carbon fatty acid features that it includes such steps as,
s1, conveying plant acidified oil and water to a pressurizing hydrolysis device, and introducing high-pressure steam to perform heating treatment to obtain crude fatty acid mixed solution;
s2, sending the crude fatty acid mixed solution obtained in the step S1 into a separation and impurity removal device for separation and impurity removal treatment to obtain primary fatty acid;
the separation and impurity removal treatment comprises oil-water separation, adsorption impurity removal and solid-liquid separation;
s3, sending the primary fatty acid in the S2 into a vacuum dehydration device for vacuum dehydration treatment to obtain medium-grade fatty acid;
s4, sending the medium-grade fatty acid in the S3 into a multi-stage rectifying device for multi-stage rectifying treatment to obtain high-carbon fatty acid;
the multi-stage rectification treatment comprises a primary rectification treatment, a secondary rectification treatment and a tertiary rectification treatment, wherein the heavy component product which is not gasified in the primary rectification treatment is a raw material of the secondary rectification treatment, and the heavy component product which is not gasified in the secondary rectification treatment is a raw material of the tertiary rectification treatment; and cooling the gasified light component products in the primary rectification treatment, the secondary rectification treatment and the tertiary rectification treatment to obtain high-carbon fatty acid refined products.
2. The process for producing high-carbon fatty acid according to claim 1, wherein in S1, the mass ratio of the vegetable acidified oil to water is 1:1-1.2.
3. The process for producing a high-carbon fatty acid according to claim 1, wherein in S1, the heating treatment is performed at a pressure of 3.5MPa to 4.0MPa, a temperature of 230 ℃ to 250 ℃ and a time of 7h to 8h.
4. The process for producing high-carbon fatty acid according to claim 1, wherein in S2, the adsorption and impurity removal is carried out by adding modified calcium phosphate to an oil layer obtained by oil-water separation.
5. The process for producing high-carbon fatty acid according to claim 4, wherein the method for producing the modified calcium phosphate comprises the steps of:
s21, dissolving 2-4 parts by mass of cellulose acetate in 100-120 parts by mass of acetone to obtain a cellulose acetate solution;
dissolving 20-24 parts by mass of calcium phosphate in 130-150 parts by mass of water to obtain a calcium phosphate suspension;
s22, dropwise adding the calcium phosphate suspension liquid obtained in the S21 into a cellulose acetate solution to obtain a mixed solution;
s23, adding the mixed solution obtained in the step S22 into water at the temperature of 40-45 ℃, stirring for 30-40 min, filtering, and drying under reduced pressure to obtain the modified calcium phosphate.
6. The process for producing high-carbon fatty acid according to claim 4, wherein the mass ratio of the oil layer to the modified calcium phosphate is 1:0.1-0.12.
7. The process for producing high-carbon fatty acid according to claim 1, wherein in S3, the temperature of the vacuum dehydration treatment is 160 ℃ to 230 ℃; the vacuum degree is 90KPa-100KPa; the time is 5min-40min.
8. The process for producing high-carbon fatty acid according to claim 1, wherein in S4, the reaction temperature of the primary rectification process is 350 ℃ to 380 ℃ and the vacuum degree is 2.5KPa to 3.0KPa; the reaction temperature of the secondary rectification process is 340-350 ℃ and the vacuum degree is 2.0KPa-2.5KPa; the reaction temperature of the three-stage rectification process is 330-340 ℃ and the vacuum degree is 1.5KPa-2.0KPa.
9. The production system of the high-carbon fatty acid is characterized by comprising a pressurizing hydrolysis device, a separating and impurity removing device, a vacuum dehydration device and a multistage rectifying device which are sequentially arranged;
the separation impurity removing device comprises an oil-water separation device, an adsorption impurity removing device and a solid-liquid separation device which are sequentially arranged;
the multistage rectifying device comprises a primary rectifying device, a secondary rectifying device and a tertiary rectifying device which are sequentially arranged, wherein a heavy component material outlet of the primary rectifying device is communicated with a material inlet of the secondary rectifying device through a primary heavy component pipeline, and a heavy component material outlet of the secondary rectifying device is communicated with a material inlet of the tertiary rectifying device through a secondary heavy component pipeline. The system for producing high-carbon fatty acid according to claim 9, wherein the primary rectifying device comprises a primary rectifying tower and a primary hydrazine cooler; the secondary rectifying device comprises a secondary rectifying tower and a secondary hydrazine cooler; the three-stage rectifying device comprises a three-stage rectifying tower and a three-stage hydrazine cooler.
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