Continuous separation and extraction device and continuous separation and extraction method for oleic acid

Abstract

The invention relates to the technical field of separation and extraction of oleic acid, in particular to a continuous separation and extraction device and a continuous separation and extraction method of oleic acid. The invention provides a continuous separation and extraction device for oleic acid. The continuous separation and extraction device comprises a falling film heat exchanger (1), a flash tower (2), a first short-path molecular distiller (4) and a second short-path molecular distiller (8) which are connected in sequence, a tower body of the first short-path molecular distiller (4) is divided into a first temperature control section (4-1), a second temperature control section (4-2) and a third temperature control section (4-3) from top to bottom; and the tower body of the second short-path molecular distiller (8) is divided into a fourth temperature control section (8-1) and a fifth temperature control section (8-2) from top to bottom. The continuous separation and extraction device can realize continuous extraction of high-quality oleic acid and meet the quality requirement of the oleic acid derivative product synthesis field on the oleic acid.

Description

Technical Field

[0001] The invention relates to the technical field of separation and extraction of oleic acid, and in particular to a continuous separation and extraction device and a continuous separation and extraction method of oleic acid. Background Art

[0002] Oleic acid is a widely used basic chemical raw material derived from animal and plant oils and fats. It can be used in plastics, resins, mineral processing, food, medicine, cosmetics, lubricants and other industries. Although production capacity and market demand have increased significantly, it is still in a homogenization development stage. There is a lack of high-quality oleic acid with good color and stability that can meet the requirements of oleic acid derivative synthesis, as well as economical and applicable separation and extraction technology. The industrial separation and extraction methods of oleic acid mainly include freeze pressing and high-tower high-temperature distillation. However, the freeze pressing method has the problems of long process, high labor intensity, low yield, high cost and difficulty in quality control. The high-tower high-temperature distillation method has the problems of high distillation temperature, high energy consumption, dark product color and poor stability. Both methods meet the quality requirements of oleic acid in the field of oleic acid derivative synthesis. Summary of the invention

[0003] In view of this, an object of the present invention is to provide a continuous separation and extraction device and a continuous separation and extraction method for oleic acid, wherein the continuous separation and extraction device can realize continuous extraction of high-quality oleic acid and meet the quality requirements of oleic acid in the field of oleic acid derivative product synthesis.

[0004] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0005] The present invention provides a continuous separation and extraction device for oleic acid, comprising a falling film heat exchanger 1, a flash tower 2, a first short-range molecular distiller 4 and a second short-range molecular distiller 8 connected in sequence;

[0006] The tower body of the first short-path molecular distiller 4 is divided from top to bottom into a first temperature control section 4-1, a second temperature control section 4-2 and a third temperature control section 4-3;

[0007] The tower body of the second short-path molecular distiller 8 is divided into a fourth temperature control section 8-1 and a fifth temperature control section 8-2 from top to bottom.

[0008] Preferably, the falling film heat exchanger 1 is provided with tubes, the upper part of the tubes is provided with a material distributor 1.1, and the tubes are connected with the material distributor 1.1;

[0009] A heat transfer oil inlet 1 - 1 is provided at the lower portion of the side wall of the falling film heat exchanger 1 .

[0010] Preferably, a gas-liquid separator 2.1 is provided in the upper part of the flash tower 2;

[0011] A liquid level gauge 2.2 is provided at the lower part of the flash tower 2, and a first discharge port 2-1 is provided at the bottom of the flash tower 2; the liquid level gauge 2.2 controls the discharge of the first discharge port 2-1 and maintains the balance of inlet and outlet in the flash tower 2;

[0012] A fatty acid delivery pump 3 is also provided between the flash tower 2 and the first short-path molecular distillation tower 4 .

[0013] Preferably, a fatty acid material receiving tank 5 and a fatty acid material delivery pump 7 are sequentially connected between the first short-path molecular distillation tower 4 and the second short-path molecular distillation tower 8 .

[0014] Preferably, the bottom of the first short-path molecular distillation tower 4 is also connected to a soft fatty acid receiving tank 6;

[0015] The first short-path molecular distillation tower 4 is provided with a first built-in condenser 4.1 inside.

[0016] Preferably, a second built-in condenser 8.1 is provided inside the second short-path molecular distillation tower 8;

[0017] The second short-path molecular distillation tower 8 is also connected to a heavy component receiving tank 9 and an oleic acid receiving tank 10, respectively.

[0018] The present invention also provides a method for continuous separation and extraction of oleic acid, which is carried out in the continuous separation and extraction device described in the above technical solution, and comprises the following steps:

[0019] After the fatty acid is heated by a falling film heat exchanger 1, it is flash evaporated by a flash tower 2 to obtain a fatty acid output;

[0020] The fatty acid output is sequentially distilled through the first temperature control section 4-1, the second temperature control section 4-1 and the third temperature control section 4-3 in the first short-path molecular distiller 4 to obtain a fatty acid output having more than 16 carbon atoms;

[0021] The fatty acid with carbon atoms greater than 16 is distilled in the fourth temperature control section 8-1 and the fifth temperature control section 8-2 in the second short-path molecular distiller 8 to obtain oleic acid.

[0022] Preferably, the acid value of the fatty acid is 200-208 mg KOH / g, the saponification value is 201-209 mg KOH / g, the iodine value is 60-7512 mg KOH / g, the mass percentage of oleic acid (C18:1) is ≥55%, and the total mass percentage of linoleic acid (C18:2) and linolenic acid (C18:3) is ≤12%;

[0023] The temperature of the flash tower 2 is 150-165° C., and the vacuum degree is 1600-2200 Pa.

[0024] Preferably, the temperature of the first temperature control section 4-1 is 156-166°C, the temperature of the second temperature control section 4-2 is 165-175°C, and the temperature of the third temperature control section 4-3 is 168-180°C;

[0025] The vacuum degree of the first short-path molecular distiller 4 is ≤20Pa.

[0026] Preferably, the temperature of the fourth temperature control section 8-1 is 180-190°C, and the temperature of the fifth temperature control section 8-2 is 185-195°C;

[0027] The vacuum degree of the second short-path molecular distiller 8 is ≤10Pa.

[0028] The present invention provides a continuous separation and extraction device for oleic acid, comprising a falling film heat exchanger 1, a flash tower 2, a first short-range molecular distiller 4 and a second short-range molecular distiller 8 connected in sequence; the tower body of the first short-range molecular distiller 4 is divided into a first temperature control section 4-1, a second temperature control section 4-2 and a third temperature control section 4-3 from top to bottom; the tower body of the second short-range molecular distiller 8 is divided into a fourth temperature control section 8-1 and a fifth temperature control section 8-2 from top to bottom. The continuous separation and extraction device of the present invention can realize segmented extraction and separation by performing segmented temperature control on the first short-range molecular distiller and the second short-range molecular distiller, thereby ensuring that the extraction efficiency of the separated oleic acid is high and can meet the quality requirements of oleic acid in the field of synthesis of oleic acid derivatives. The oleic acid separated by the separation and extraction device is better than the industry standard (OB / T2153-2010). BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 This is a schematic structural diagram of the continuous separation and extraction device for oleic acid according to the present invention;

[0030] Among them, 1 is a falling film heat exchanger, 1-1 is a first heat transfer oil inlet, 1-2 is a raw material inlet, 1-3 is a first heat transfer oil outlet, 1.1 is a material distributor, 2 is a flash tower, 2-1 is a first discharge port, 2.1 is a gas-liquid separator, 2.2 is a liquid level meter, 2.3 is a first vacuum port, 3 is a fatty acid delivery pump, 4 is a first short-range molecular distiller, 4-1 is a first temperature control section, 4-2 is a second temperature control section, 4-3 is a third temperature control section, 4-4 is a first feed port, 4-5 is a second heat transfer oil inlet, 4-6 is a second heat transfer oil outlet, 4-7 is a third heat transfer oil inlet, 4-8 is a third heat transfer oil outlet, 4-9 is a fourth heat transfer oil inlet, 4-10 is a fourth heat transfer oil outlet, and 4-11 is a fifth heat transfer oil outlet. three heat transfer oil outlets, 4.1 is the first built-in condenser, 4.2 is the first cooling water inlet, 4.3 is the first cooling water outlet, 4.4 is the second vacuum port, 5 is the fatty acid material receiving tank, 6 is the soft fatty acid receiving tank, 7 is the fatty acid material delivery pump, 8 is the second short-range molecular distiller, 8-1 is the fourth temperature control section, 8-2 is the fifth temperature control section, 8-3 is the second feed port, 8-4 is the fifth heat transfer oil inlet, 8-5 is the fifth heat transfer oil outlet, 8-6 is the sixth heat transfer oil inlet, 8-7 is the sixth heat transfer oil outlet, 8.1 is the second built-in condenser, 8.2 is the second cooling water inlet, 8.3 is the second cooling water outlet, 9 is the heavy component receiving tank, and 10 is the oleic acid receiving tank. DETAILED DESCRIPTION

[0031] The present invention provides a continuous separation and extraction device for oleic acid, comprising a falling film heat exchanger 1, a flash tower 2, a first short-range molecular distiller 4 and a second short-range molecular distiller 8 connected in sequence;

[0032] The tower body of the first short-path molecular distiller 4 is divided from top to bottom into a first temperature control section 4-1, a second temperature control section 4-2 and a third temperature control section 4-3;

[0033] The tower body of the second short-path molecular distiller 8 is divided into a fourth temperature control section 8-1 and a fifth temperature control section 8-2 from top to bottom.

[0034] As an embodiment of the present invention, the falling film heat exchanger 1 is a shell-and-tube falling film heat exchanger, and the heat exchange area F of the shell-and-tube falling film heat exchanger is preferably 30m 2 ; The falling film heat exchanger 1 is provided with uniformly distributed tubes, and a material distributor 1.1 is installed on the upper part of the tubes. The tubes are connected to the material distributor 1.1 so as to evenly distribute the fatty acid raw materials into each tube and form a film in the tube to flow continuously from top to bottom along the inner wall; The first heat transfer oil inlet 1-1 is provided at the lower part of the side wall of the falling film heat exchanger 1.

[0035] As an embodiment of the present invention, a raw material inlet 1-2 is also provided at the top of the falling film heat exchanger 1. A first heat transfer oil outlet 1-3 is provided above the side wall of the falling film heat exchanger 1, and the level of the first heat transfer oil outlet 1-3 is lower than the level of the material distributor 1.1. A first heat transfer oil inlet 1-1 is provided below the side wall of the falling film ventilator, and the level of the first heat transfer oil inlet 1-1 is higher than the level of the bottom of the tube array.

[0036] In the present invention, the fatty acid enters into the tubes of the tube array through the material distributor 1.1, forms a film in the tube, flows continuously from top to bottom along the inner wall, and is heated by the heat transfer oil outside the tube array.

[0037] As an embodiment of the present invention, a gas-liquid separator 2.1 is provided in the upper part of the flash tower 2; a liquid level meter 2.2 is provided in the lower part of the flash tower 2, and a first discharge port 2-1 is provided at the bottom of the flash tower 2; the liquid level meter 2.2 controls the discharge of the first discharge port 2-1 and maintains the balance of the inlet and outlet of the flash tower 2; a fatty acid delivery pump 3 is also provided between the flash tower 2 and the first short-range molecular distillation tower 4, and a first feed port 4-4 is provided at the top of the first short-range molecular distillation tower 4; the first discharge port 2-1, the fatty acid delivery pump 3 and the first feed port 4-4 are connected in sequence. A first vacuum port 2.3 is also provided at the top of the flash tower.

[0038] As an embodiment of the present invention, the barrel size of the flash tower 2 is Φ / 1000×H1500mm.

[0039] In the present invention, the gas-liquid separator 2.1 can remove gas, water and colored, odorous and volatile substances in the fatty acid raw material from the top of the tower.

[0040] As an embodiment of the present invention, the first short-range molecular distiller 4 is preferably a rotary scraped film short-range molecular distiller with an evaporation area of ​​F=25m 2, the inner cylinder diameter Φ=1400mm, the inner cylinder scraping speed is preferably 40-80 rpm, which is adjusted and controlled by the frequency converter. The tower body of the first short-range molecular distiller 4 is divided into a first temperature control section 4-1, a second temperature control section 4-2 and a third temperature control section 4-3 from top to bottom. A second heat transfer oil inlet 4-5 is provided below the side wall of the first temperature control section 4-1, and a second heat transfer oil outlet 4-6 is provided above the side wall of the first temperature control section 4-1; a third heat transfer oil inlet 4-7 is provided below the side wall of the second temperature control section 4-2, and a third heat transfer oil outlet 4-8 is provided above the side wall of the second temperature control section 4-2; a fourth heat transfer oil inlet 4-9 is provided below the side wall of the third temperature control section 4-3, and a third heat transfer oil outlet 4-10 is provided above the side wall of the third temperature control section 4-3. In the present invention, the first short-range molecular distiller 4 controls the distillation temperature separately in sections, so that fatty acids of different chain lengths can be distilled in sections.

[0041] As an embodiment of the present invention, the bottom of the first short-range molecular distillation tower 4 is also connected to a soft fatty acid receiving tank 6; the first short-range molecular distillation tower 4 is provided with a first built-in condenser 4.1, which is preferably a U-shaped shell-and-tube condenser with a heat exchange area of ​​80 to 120 m 2 The distance between the inner cylinder evaporation surface of the first short-range molecular distillation tower 4 and the condensation surface of the first built-in condenser 4.1 is preferably 80 to 100 mm. The first built-in condenser 4.1 is also provided with a first cooling water inlet 4.2 and a first cooling water outlet 4.3 at the bottom of the first short-range molecular distillation tower 4. The side wall bottom of the first short-range molecular distillation tower 4 is also provided with a second vacuum port 4.4.

[0042] As an embodiment of the present invention, a fatty acid material receiving tank 5 and a fatty acid material delivery pump 7 are sequentially connected between the first short-range molecular distillation tower 4 and the second short-range molecular distillation tower 8, and the fatty acid material delivery pump 7 is connected to a second feed port 8-3 arranged at the top of the second short-range molecular distillation tower 8. A flow meter is installed on the connecting pipeline between the first short-range molecular distillation tower 4, the fatty acid material receiving tank 5, the fatty acid material delivery pump 7 and the second short-range molecular distillation tower 8 to display the flow rate of the controlled material.

[0043] As an embodiment of the present invention, the second short-range molecular distiller 8 is preferably a rotary scraped film short-range molecular distiller with an evaporation area of ​​F=20m 2, the inner cylinder diameter Φ=1500mm, the inner cylinder scraping speed is preferably 30-90 rpm, which is adjusted and controlled by the frequency converter. The tower body of the second short-range molecular distiller 8 is divided into a fourth temperature control section 8-1 and a fifth temperature control section 8-2 from top to bottom; a fifth heat transfer oil inlet 8-4 is provided below the side wall of the fourth temperature control section 8-1, and a fifth heat transfer oil outlet 8-5 is provided above the side wall of the fourth temperature control section 8-1; a sixth heat transfer oil inlet 8-6 is provided below the side wall of the fifth temperature control section 8-2, and a sixth heat transfer oil outlet 8-7 is provided above the side wall of the fifth temperature control section 8-2. In the present invention, the second short-range molecular distillation tower controls the distillation temperature separately to ensure the yield and quality of oleic acid.

[0044] As an embodiment of the present invention, the second short-range molecular distillation tower 8 is provided with a second built-in condenser 8.1, which is preferably a U-shaped shell-and-tube condenser with a heat exchange area of ​​60 to 80 m 2 The distance between the inner cylinder evaporation surface of the second short-range molecular distillation tower 8 and the condensation surface of the second built-in condenser 8.1 is preferably 60 to 90 mm. The second built-in condenser 8.1 is also provided with a second cooling water inlet 8.2 and a second cooling water outlet 8.3 at the bottom of the second short-range molecular distillation tower 8. The side wall bottom of the second short-range molecular distillation tower 8 is also provided with a third vacuum port 8.4.

[0045] As an embodiment of the present invention, the second short-path molecular distillation tower 8 is further connected to a heavy component receiving tank 9 and an oleic acid receiving tank 10, respectively.

[0046] As an embodiment of the present invention, the fatty acid delivery pump 3 and the fatty acid material delivery pump 7 are high-precision gear pumps (mark pumps) and are equipped with variable frequency speed regulators. In the embodiment of the present invention, the flow rates of the fatty acid delivery pump 3 and the fatty acid material delivery pump 7 are preferably 1 to 1.6 m / s. 3 In the present invention, the above-mentioned arrangement of the fatty acid delivery pump 3 and the fatty acid material delivery pump 7 can well regulate and control the flow rate of the transported materials to ensure smooth operation.

[0047] As an embodiment of the present invention, the first heat transfer oil inlet 1-1, the second heat transfer oil inlet 4-5, the third heat transfer oil inlet 4-7, the fourth heat transfer oil inlet 4-9, the fifth heat transfer oil inlet 8-4 and the sixth heat transfer oil inlet 8-6 are all automatically regulated and controlled by the regulating valve interlock.

[0048] The present invention also provides a method for continuous separation and extraction of oleic acid, which is carried out in the continuous separation and extraction device described in the above technical solution, and comprises the following steps:

[0049] After the fatty acid is heated by a falling film heat exchanger 1, it is flash evaporated by a flash tower 2 to obtain a fatty acid output;

[0050] The fatty acid output is sequentially distilled through the first temperature control section 4-1, the second temperature control section 4-1 and the third temperature control section 4-3 in the first short-path molecular distiller 4 to obtain a fatty acid output having more than 16 carbon atoms;

[0051] The fatty acid with carbon atoms greater than 16 is distilled in the fourth temperature control section 8-1 and the fifth temperature control section 8-2 in the second short-path molecular distiller 8 to obtain oleic acid.

[0052] In the present invention, the fatty acid is heated by a falling film heat exchanger 1 and then flashed by a flash tower 2 to obtain a fatty acid output material.

[0053] In the present invention, the acid value of the fatty acid is preferably 200-208 mg KOH / g, the saponification value is preferably 201-209 mg KOH / g, the iodine value is preferably 60-7512 mg KOH / g, the mass percentage of oleic acid (C18:1) is preferably ≥55%, and the total mass percentage of linoleic acid (C18:2) and linolenic acid (C18:3) is preferably ≤12%.

[0054] In the present invention, the temperature of the flash tower 2 is preferably 150-165° C., and the vacuum degree is preferably 1600-2200 Pa. In the present invention, controlling the above conditions in the flash tower 2 can remove gas, water and colored and odorous volatiles in fatty acids from the top of the tower.

[0055] After obtaining the fatty acid output, the present invention distills the fatty acid output in sequence through the first temperature control section 4-1, the second temperature control section 4-1 and the third temperature control section 4-3 in the first short-range molecular distiller 4 to obtain a fatty acid output with more than 16 carbon atoms.

[0056] In the present invention, the temperature of the first temperature control section 4-1 is preferably 156-166° C., the temperature of the second temperature control section 4-2 is preferably 165-175° C., and the temperature of the third temperature control section 4-3 is preferably 168-180° C. The vacuum degree of the first short-range molecular distiller 4 is preferably ≤20Pa.

[0057] In the present invention, by controlling the temperature of the first temperature control section within the above range, fatty acids with a temperature of ≤12°C can be evaporated and separated cleanly; by controlling the temperature of the second temperature control section within the above range, fatty acids with a temperature of ≤14°C can be evaporated and separated cleanly; by controlling the temperature of the third temperature control section within the above range, fatty acids with a temperature of ≤16°C can be evaporated and separated cleanly.

[0058] After obtaining the fatty acid output with more than 16 carbon atoms, the present invention distills the fatty acid output with more than 16 carbon atoms through the fourth temperature control section 8-1 and the fifth temperature control section 8-2 in the second short-path molecular distiller 8 in sequence to obtain oleic acid.

[0059] In the present invention, the temperature of the fourth temperature control section 8-1 is preferably 180-190°C, and the temperature of the fifth temperature control section 8-2 is preferably 185-195°C; the vacuum degree of the second short-range molecular distiller 8 is preferably ≤10Pa.

[0060] In the present invention, the temperature of the fourth temperature control section 8-1 and the temperature of the fifth temperature control section 8-2 are controlled within the above ranges to separate fatty acids greater than 18C from oleic acid.

[0061] The technical solutions in the present invention will be described clearly and completely below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0062] Example 1

[0063] like Figure 1 As shown, the continuous separation and extraction device of oleic acid comprises a falling film heat exchanger 1, a flash tower 2, a first short-range molecular distiller 4 and a second short-range molecular distiller 8 connected in sequence; the tower body of the first short-range molecular distiller 4 is divided into a first temperature control section 4-1, a second temperature control section 4-2 and a third temperature control section 4-3 from top to bottom; the tower body of the second short-range molecular distiller 8 is divided into a fourth temperature control section 8-1 and a fifth temperature control section 8-2 from top to bottom; the falling film heat exchanger 1 is a shell-and-tube falling film heat exchanger, and the heat exchange area F of the shell-and-tube falling film heat exchanger is 30m 2The falling film heat exchanger 1 is provided with tubes, and a material distributor 1.1 is installed on the upper part of the tubes, and the tubes are connected with the material distributor 1.1; the lower part of the side wall of the falling film heat exchanger 1 is provided with a first heat transfer oil inlet 1-1; the top of the falling film heat exchanger 1 is also provided with a raw material inlet 1-2. A first heat transfer oil outlet 1-3 is provided above the side wall of the falling film heat exchanger 1, and the level of the first heat transfer oil outlet 1-3 is lower than the level of the material distributor 1.1. A first heat transfer oil inlet 1-1 is arranged below the side wall of the falling film ventilator, and the horizontal height of the first heat transfer oil inlet 1-1 is higher than the horizontal height of the bottom of the tube; the barrel size of the flash tower 2 is Φ / 1000×H1500mm; a gas-liquid separator 2.1 is arranged at the upper part of the flash tower 2; a liquid level gauge 2.2 is arranged at the lower part of the flash tower 2, and a first discharge port 2-1 is arranged at the bottom of the flash tower 2; the liquid level gauge 2.2 controls the discharge of the first discharge port 2-1 and maintains the balance of feed and discharge in the flash tower 2; a fatty acid delivery pump 3 is also arranged between the flash tower 2 and the first short-range molecular distillation tower 4, and a first feed port 4-4 is arranged at the top of the first short-range molecular distillation tower 4; the first discharge port 2-1, the fatty acid delivery pump 3 and the first feed port 4-4 are connected in sequence. The top of the flash tower is also provided with a first vacuum port 2.3; the first short-range molecular distiller 4 is a rotary scraped film short-range molecular distiller with an evaporation area of ​​F=25m 2 , the inner cylinder diameter Φ=1400mm, the inner cylinder scraping speed is 40-80 rpm, which is adjusted and controlled by the frequency converter; the tower body of the first short-range molecular distiller 4 is divided into a first temperature control section 4-1, a second temperature control section 4-2 and a third temperature control section 4-3 from top to bottom. A second heat transfer oil inlet 4-5 is provided below the side wall of the first temperature control section 4-1, and a second heat transfer oil outlet 4-6 is provided above the side wall of the first temperature control section 4-1; a third heat transfer oil inlet 4-7 is provided below the side wall of the second temperature control section 4-2, and a third heat transfer oil outlet 4-8 is provided above the side wall of the second temperature control section 4-2; a fourth heat transfer oil inlet 4-9 is provided below the side wall of the third temperature control section 4-3, and a third heat transfer oil outlet 4-10 is provided above the side wall of the third temperature control section 4-3; the bottom of the first short-range molecular distillation tower 4 is also connected to a soft fatty acid receiving tank 6; the first short-range molecular distillation tower 4 is provided with a first built-in condenser 4.1 inside, and the first built-in condenser 4.1 is a U-shaped shell and tube condenser with a heat exchange area of ​​F=92m 2. The distance between the inner cylinder evaporation surface of the first short-range molecular distillation tower 4 and the condensation surface of the first built-in condenser 4.1 is 95mm; the first built-in condenser 4.1 is also provided with a first cooling water inlet 4.2 and a first cooling water outlet 4.3 at the bottom of the first short-range molecular distillation tower 4. The side wall bottom of the first short-range molecular distillation tower 4 is also provided with a second vacuum port 4.4; the fatty acid material receiving tank 5 and the fatty acid material delivery pump 7 are also connected in sequence between the first short-range molecular distillation tower 4 and the second short-range molecular distillation tower 8, and the fatty acid material delivery pump 7 is connected to the second feed port 8-3 arranged at the top of the second short-range molecular distillation tower 8; the connecting pipeline between the first short-range molecular distillation tower 4, the fatty acid material receiving tank 5, the fatty acid material delivery pump 7 and the second short-range molecular distillation tower 8 is equipped with a flow meter for displaying and controlling the flow of the material; the second short-range molecular distillation tower 8 is a rotary scraped film short-range molecular distillation tower, and the evaporation area F=20m 2 , the inner cylinder diameter Φ = 1500mm, the inner cylinder scraping speed is 45 rpm, which is adjusted and controlled by the frequency converter; the tower body of the second short-range molecular distillation tower 8 is divided into a fourth temperature control section 8-1 and a fifth temperature control section 8-2 from top to bottom; a fifth heat transfer oil inlet 8-4 is arranged below the side wall of the fourth temperature control section 8-1, and a fifth heat transfer oil outlet 8-5 is arranged above the side wall of the fourth temperature control section 8-1; a sixth heat transfer oil inlet 8-6 is arranged below the side wall of the fifth temperature control section 8-2, and a sixth heat transfer oil outlet 8-7 is arranged above the side wall of the fifth temperature control section 8-2; a second built-in condenser 8.1 is arranged inside the second short-range molecular distillation tower 8, and the second built-in condenser 8.1 is a U-shaped shell and tube condenser with a heat exchange area of ​​F = 75m 2 . The distance between the inner cylinder evaporation surface of the second short-range molecular distillation tower 8 and the condensation surface of the second built-in condenser 8.1 is 82 mm; the second built-in condenser 8.1 is also provided with a second cooling water inlet 8.2 and a second cooling water outlet 8.3 at the bottom of the second short-range molecular distillation tower 8. A third vacuum port 8.4 is also provided at the bottom of the side wall of the second short-range molecular distillation tower 8; the second short-range molecular distillation tower 8 is also connected to a heavy component receiving tank 9 and an oleic acid receiving tank 10 respectively; the fatty acid delivery pump 3 and the fatty acid material delivery pump 7 are high-precision gear pumps (mark pumps) and are equipped with variable frequency speed regulators; the flow rate of the fatty acid delivery pump 3 and the fatty acid material delivery pump 7 is 1.3m 3 The first heat transfer oil inlet 1-1, the second heat transfer oil inlet 4-5, the third heat transfer oil inlet 4-7, the fourth heat transfer oil inlet 4-9, the fifth heat transfer oil inlet 8-4 and the sixth heat transfer oil inlet 8-6 are all automatically regulated and controlled by the regulating valve interlock.

[0064] Continuous separation and extraction method of oleic acid: the fatty acid (acid value is 202.3 mg·KOH / g, saponification value is 203.2 mg·KOH / g, iodine value is 68.2I2·mg·KOH / g, C18:1 mass percentage ≥58.1%, C18:2+C18:3 total mass percentage ≤10.9%) is heated by a falling film heat exchanger 1, and flashed by a flash tower 2 (the flash temperature is 158-162°C, and the vacuum degree is 1800Pa) to obtain a fatty acid output; the fatty acid output is sequentially distilled by the first temperature control section 4-1 (temperature is 160-163°C), the second temperature control section 4-1 (temperature is 166-169°C) and the third temperature control section 4-3 (temperature is 172-175°C) in the first short-range molecular distiller 4 (vacuum degree is 12Pa) to obtain a fatty acid output having more than 16 carbon atoms; the The fatty acid with more than 16 carbon atoms is distilled in the fourth temperature control section 8-1 (temperature of 184-186° C.) and the fifth temperature control section 8-2 (temperature of 189-193° C.) in the second short-path molecular distiller 8 (vacuum degree of 6 Pa) to obtain oleic acid (color 45-50 Hazen, heating stability (180° C. / 2h) 480-500 Hazen, acid value 201.2-202.3 mg· The quality is very stable, which is significantly better than the industry standard QB / T2153-2010 (color 200Hazen, iodine value 80~102I2·mg·KOH / g, acid value 190~203mg·KOH / g, saponification value 190~205mg·KOH / g).

[0065] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A continuous separation and extraction device for oleic acid, characterized in that: It comprises a falling film heat exchanger (1), a flash tower (2), a first short-path molecular distiller (4) and a second short-path molecular distiller (8) which are connected in sequence; The tower body of the first short-path molecular distiller (4) is divided from top to bottom into a first temperature control section (4-1), a second temperature control section (4-2) and a third temperature control section (4-3); The tower body of the second short-path molecular distiller (8) is divided from top to bottom into a fourth temperature control section (8-1) and a fifth temperature control section (8-2).

2. The continuous separation and extraction device according to claim 1, characterized in that: The falling film heat exchanger (1) is provided with a tube array, a material distributor (1.1) is installed on the upper part of the tube array, and the tube array is connected to the material distributor (1.1); A heat transfer oil inlet (1-1) is provided at the lower part of the side wall of the falling film heat exchanger (1).

3. The continuous separation and extraction device according to claim 1, characterized in that: A gas-liquid separator (2.1) is provided in the upper part of the flash tower (2); A liquid level meter (2.2) is provided at the lower part of the flash tower (2), and a first discharge port (2-1) is provided at the bottom of the flash tower (2); the liquid level meter (2.2) controls the discharge of the first discharge port (2-1) and maintains the balance of the inlet and outlet of the flash tower (2); A fatty acid delivery pump (3) is also provided between the flash tower (2) and the first short-path molecular distillation tower (4).

4. The continuous separation and extraction device according to claim 1, characterized in that: A fatty acid material receiving tank (5) and a fatty acid material delivery pump (7) are sequentially connected between the first short-path molecular distillation tower (4) and the second short-path molecular distillation tower (8).

5. The continuous separation and extraction device according to claim 1 or 4, characterized in that: The bottom of the first short-path molecular distillation tower (4) is also connected to a soft fatty acid receiving tank (6); A first built-in condenser (4.1) is arranged inside the first short-path molecular distillation tower (4).

6. The continuous separation and extraction device according to claim 1 or 4, characterized in that: A second built-in condenser (8.1) is provided inside the second short-path molecular distillation tower (8); The second short-path molecular distillation tower (8) is also connected to a heavy component receiving tank (9) and an oleic acid receiving tank (10), respectively.

7. A method for continuous separation and extraction of oleic acid, characterized in that: The continuous separation and extraction method of oleic acid is carried out in the continuous separation and extraction device according to any one of claims 1 to 6, comprising the following steps: The fatty acid is heated by a falling film heat exchanger (1), and then flashed by a flash tower (2) to obtain a fatty acid output; The fatty acid output is sequentially distilled through the first temperature control section (4-1), the second temperature control section (4-2) and the third temperature control section (4-3) in the first short-path molecular distiller (4) to obtain a fatty acid output having more than 16 carbon atoms; The fatty acid with carbon atoms greater than 16 is distilled in the fourth temperature control section (8-1) and the fifth temperature control section (8-2) of the second short-path molecular distiller (8) to obtain oleic acid.

8. The continuous separation and extraction method according to claim 7, characterized in that: The fatty acid has an acid value of 200-208 mg KOH / g, a saponification value of 201-209 mg KOH / g, an iodine value of 60-7512 mg KOH / g, a mass percentage of oleic acid ≥ 55%, and a total mass percentage of linoleic acid and linolenic acid ≤ 12%; The temperature of the flash tower (2) is 150-165°C, and the vacuum degree is 1600-2200Pa.

9. The continuous separation and extraction method according to claim 7, characterized in that: The temperature of the first temperature control section (4-1) is 156-166°C, the temperature of the second temperature control section (4-2) is 165-175°C, and the temperature of the third temperature control section (4-3) is 168-180°C; The vacuum degree of the first short-path molecular distiller (4) is ≤20Pa.

10. The continuous separation and extraction method according to claim 7, characterized in that: The temperature of the fourth temperature control section (8-1) is 180-190°C, and the temperature of the fifth temperature control section (8-2) is 185-195°C; The vacuum degree of the second short-path molecular distiller (8) is ≤10Pa.

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