CN113198199A

CN113198199A - Method for removing odor substances in prickly ash seed oil and wiped film type molecular distillation device used in method

Info

Publication number: CN113198199A
Application number: CN202110654524.2A
Authority: CN
Inventors: 黄涛; 米涛; 王黔林; 陆龙发; 梁世康
Original assignee: Guizhou Xuande Biotechnology Co ltd
Current assignee: Guizhou Xuande Biotechnology Co ltd
Priority date: 2021-06-11
Filing date: 2021-06-11
Publication date: 2021-08-03

Abstract

The invention discloses a method for removing odor substances in prickly ash seed oil and a wiped film type molecular distillation device used in the method. For the wiped film type molecular distillation device, a great factor influencing the separation effect is found in the use process, namely the effective separation rate is low due to the fact that mist caused by rotation of the scraper directly contacts with the condensing pipe, the technology of the wiped film type molecular distillation device cannot be popularized to large-scale production, and the applicant improves the wiped film type molecular distillation device to overcome the defects of the existing wiped film type molecular distillation device.

Description

Method for removing odor substances in prickly ash seed oil and wiped film type molecular distillation device used in method

Technical Field

The invention relates to a method for removing odor substances from prickly ash seed oil and a wiped film type molecular distillation device used by the method, and belongs to the grain and oil processing technology in the field of food.

Background

The prickly ash seed oil is prepared by using byproduct prickly ash seed kernels of prickly ash as a raw material and refining the raw material through a modern oil production process and advanced equipment, and the main components of the prickly ash seed oil are palmitic acid, palmitoleic acid, stearic acid, oleic acid, linoleic acid and linolenic acid. The pricklyash seed oil is a high-grade health edible oil rich in alpha-linolenic acid, which is polyunsaturated fatty acid essential for human body, is an important component for forming human tissue cells, and is a substance essential for human health.

The production method of the crude oil of the pepper seeds comprises the processes of squeezing, leaching by an organic solvent, extracting by supercritical CO2 and the like, but the crude oil of the pepper seeds has the characteristics of high acid value, dark color, poor taste and the like, can not be directly eaten, and needs to be subjected to deacidification, decoloration and deodorization treatment. At present, the stink substances in the prickly ash seed oil are removed mainly by steam distillation deodorization, the deodorization temperature is up to 240 ℃, and the heat-sensitive substances are easy to be oxidized and decomposed at high temperature. The working principle is that the separated liquid is mostly uniformly distributed on the inner wall of the cylinder body in an overflow mode, and then is stricken off by a rotating scraper to form a liquid film with a certain thickness, so that the molecular motion of the molecular distillation process is better formed, and the separation of heavy components and light components is realized; however, the existing wiped film type molecular distillation device has the following problems:

1, because the installed equipment is difficult to ensure to be completely horizontal, firstly, the overflow liquid has liquid quantity difference, further, a part of liquid film is thicker, and a part of area is thinner, so that the separation of heavy components and light components has certain influence;

2 because the scraper of the existing scraper type molecular distillation device has a high rotating speed, when the scraper meets a liquid flow with a large amount, the phenomenon of spray splashing is easily aggravated, the spray contacts with a condensation surface to influence the separation effect, and the rotating speed of the common scraper is high for realizing large-scale production, but the yield is low, and the common scraper cannot be used in a good industrialized way;

3 in the large-scale production process, the scraper blade is more easily worn and torn as flexible friction piece, and the doctor-bar on the scraper blade of current is the strip, is compressed tightly by the bolt more, and the bolt need loosen one by one in the change, and the maintenance speed is slower and easily pollute the jar body.

Disclosure of Invention

The invention aims to provide a method for removing odor substances in prickly ash seed oil and a wiped film type molecular distillation device used by the method, which can well overcome the defects in the prior art.

In order to achieve the purpose, the invention adopts the following technical scheme:

the method for removing the odor substances in the prickly ash seed oil is to distill the pretreated prickly ash seed oil by utilizing molecular distillation equipment, remove the odor substances from a light phase and obtain a finished product of prickly ash seed oil from a heavy phase.

The method for removing the odor substances in the pricklyash seed oil comprises the steps of performing deacidification and decoloration treatment on the pricklyash seed crude oil, wherein the acid value of the treated pricklyash seed oil is less than 3.0 (KOH)/(mg/g); the crude oil of pepper seeds is prepared by squeezing pepper seeds and extracting by supercritical CO 2.

The method for removing the odor substances in the prickly ash seed oil comprises the steps that the distillation equipment is a wiped film type molecular distillation device, the distillation temperature of the wiped film type molecular distillation device is set to be 160-200 ℃, the rotating speed of a heating oil preheating wiped film device is 10-15 r/min, and the vacuum degree is-0.04-0.09 MPa.

A wiped film type molecular distillation device for removing odor substances in prickly ash seed oil comprises a cylinder body provided with a jacket, a heating oil circulating system is connected on a jacket of the cylinder body, a condensing pipe is arranged in the cylinder body, a water cooling circulating system is connected on the condensing pipe, a vacuumizing device is arranged on the cylinder body, a heavy component collecting port is arranged at the bottom of the cylinder body and is connected with a heavy component collecting tank, a light component collecting tank is sleeved at the bottom of the condensing pipe, a light component discharge port is arranged on the light component collecting tank and connected with a light component collecting tank, a motor is arranged on the cylinder body, a material distribution disc is arranged in the cylinder body, an output shaft of the motor is connected with the circle center of the material distribution disc, one or two notches are arranged on the material distribution disc, the bottom surface of the material distribution disc at the notch is contacted with the inner wall of the cylinder body, a scraping plate is connected on the material distribution disc, and the scraping plate of the scraping plate is in clearance fit with the inner wall of the cylinder body.

The scraping film type molecular distillation device for removing the odor substances in the prickly ash seed oil is characterized in that the scraping plate is composed of 2-4 sections of scraping sheets, the 2-4 sections of scraping sheets are arranged in a staggered mode from top to bottom, and every two adjacent scraping sheets are connected through a connecting plate.

The wiped film type molecular distillation device for removing odor substances in the prickly ash seed oil is characterized in that a rotary table is sleeved outside a light component collecting tank, and a scraper at the lowest part is connected with the rotary table.

The scraped molecular distillation device for removing the odor substances in the prickly ash seed oil is characterized in that 2-4 sections of scraping blades are staggered from top to bottom step by step, the positions of the notches are used as starting positions, and the scraping blades which are closer to each other pass through the starting positions faster.

The scraped molecular distillation device for removing the odor substances in the prickly ash seed oil has 2-4 sections of scraping blades with smaller gaps from top to bottom with the inner wall of the cylinder body.

The scraping film type molecular distillation device for removing odor substances in the prickly ash seed oil is characterized in that the scraping blade comprises a hard scraping strip mounting plate and a flexible scraping strip, and the scraping strip mounting plate and the scraping strip are connected in a tenon insertion mode.

Compared with the prior art, the invention utilizes molecular distillation equipment to distill the pretreated zanthoxylum seed oil, removes odor substances from the light phase, and obtains the finished zanthoxylum seed oil from the heavy phase, thereby well controlling the temperature and better ensuring that the total beneficial substances of the zanthoxylum oil are not oxidized. The distillation equipment is a wiped film type molecular distillation device, the distillation temperature of the wiped film type molecular distillation device is set to be 160-200 ℃, the rotating speed of a heating oil preheating wiped film device is 5-10 r/min, the vacuum degree is-0.04-0.09 MPa, the pepper seed oil processed under the process conditions has good taste after detection, and the product has no peculiar smell. Meanwhile, the distillation equipment structure is optimized and adjusted, so that the effective separation rate of the produced pricklyash seed oil is improved.

For the wiped film type molecular distillation device, a great factor influencing the separation effect is found in the use process, namely the effective separation rate is low due to the fact that mist caused by rotation of the scraper directly contacts with the condensing pipe, the technology of the wiped film type molecular distillation device cannot be popularized to large-scale production, and the applicant improves the wiped film type molecular distillation device to overcome the defects of the existing wiped film type molecular distillation device

1. The overflow mode of change barrel upper end, be provided with the motor on the barrel, be equipped with the branch charging tray in the barrel, the output shaft of motor is connected with the centre of a circle of branch charging tray, be equipped with one or two breachs on the branch charging tray, the bottom surface and the barrel inner wall contact of the branch charging tray of breach department, such setting can make the material get rid of on the section of thick bamboo wall under the effect of centrifugal force, and just can effectively control from the breach through the material volume in the control branch charging tray how much of leaving the material, the installation levelness that the mode can reduce equipment is overflowed to current horizontal terminal surface relatively.

The scraping plates are composed of 2-4 sections of scraping plates, the 2-4 sections of scraping plates are arranged in a staggered manner from top to bottom, and two adjacent scraping plates are connected through a connecting plate, so that the purpose of the arrangement is to better match the arrangement of an improved material distribution plate, the contact between a material liquid and a cylinder wall is not uniform material distribution due to the modified material distribution plate and the arrangement of a notch on the modified material distribution plate, so that the material slides along the cylinder wall under the action of gravity by taking the notch of the material distribution plate as a starting point in the working process, and the sliding process has certain time due to certain viscosity of the grease, so that a multi-sheet structure arranged in a stepped staggered manner can better adapt to the falling of the grease, the covering surface of a liquid film is increased, the thickness of the liquid film is reduced, and the separation effect of light components and heavy components is further improved; meanwhile, the applicant tests that the structure that 2-4 sections of scraping sheets are staggered from top to bottom step by step is adopted, the rotating speed of the scraping sheets can be reduced from the original 25-30 r/min to 10-15 r/min, the phenomenon of spray splashing can be reduced while the rotating speed is reduced, the separation effect of light components and heavy components is further improved, and the separation rate and the quality and the taste of the separated oil are ensured. Meanwhile, the abrasion of the scraper can be effectively reduced due to the reduction of the rotating speed, the continuous running time of the equipment is prolonged, and the maintenance cost is reduced

3. The 2-4 sections of the scraping blades are staggered from top to bottom step by step in a way that the position of the notch is taken as a starting position, and the scraping blades which are closer to the upper part pass through the starting position faster; the smaller the gap between the 2-4 sections of the scraping sheets and the inner wall of the cylinder from top to bottom is; the scraper comprises a hard scraping strip mounting plate and a flexible scraping strip, and the scraping strip mounting plate and the scraping strip are connected in a tenon inserting mode. The arrangement mode and the structure are further optimized and adjusted after use, and the arrangement mode of the scraper plate further improves the separation effect of light components and heavy components; the structure of sectional type can conveniently scrape the strip and adopt the mortise grafting mode to connect with the mounting panel, and it is faster to change the speed, and the staff can accomplish, and then can reduce the pollution to food level equipment.

In order to prove the improvement effect, 40kg of crude pepper seed oil prepared by a supercritical CO2 extraction process is taken by an applicant, deacidification and decoloration treatment are carried out on the prepared crude pepper seed oil to obtain pretreated pepper seed oil, the acid value of the pretreated pepper seed oil is 0.51 (KOH)/(mg/g), the pretreated pepper seed oil is uniformly divided into two parts by a liquid divider, the two parts are respectively sent to the existing wiped film type molecular distillation device and the improved wiped film type molecular distillation device, the distillation temperature is set to be 180 ℃, the vacuum degree is-0.079 MPa, the rotating speed before improvement is 30 r/min, the rotating speed after improvement is 12r/min, a comparison test is carried out, and the test results show that 1.3kg of odorous substances are obtained from the light phase of the existing wiped film type molecular distillation device and 18.5kg of finished pepper oil is obtained from the heavy phase; the improved wiped film type molecular distillation device can obtain 1.0kg of odorous substances in the light phase and 18.8kg of finished zanthoxylum oil in the heavy phase.

Drawings

FIG. 1 is a schematic structural diagram of the present invention

FIG. 2 is a schematic view of the structure of the material distribution tray, the condenser tube and the scraper thereof in the scraped molecular distillation apparatus.

Detailed Description

Example 1

A method for removing odor substances in prickly ash seed oil comprises distilling pretreated prickly ash seed oil with molecular distillation equipment, removing odor substances from light phase, and obtaining final product prickly ash seed oil from heavy phase. The pretreated pricklyash seed oil is obtained by deacidifying and decolorizing crude pricklyash seed oil, and the acid value of the treated pricklyash seed oil is less than 3.0 (KOH)/(mg/g); the crude oil of pepper seeds is prepared by squeezing pepper seeds and extracting by supercritical CO 2.

The adopted molecular distillation equipment is a wiped film type molecular distillation device, and the specific operation process is as follows:

[1] obtaining pepper seed oil pretreated by raw materials: adopting supercritical CO2 to obtain crude oil of semen Zanthoxyli, deacidifying and decolorizing, and obtaining pretreated semen Zanthoxyli oil with acid value of 0.51 (KOH)/(mg/g).

[2] Pumping the pretreated pricklyash seed oil into a feed chute of a molecular distiller, and turning on a power supply.

[3] Starting a cooling water circulating pump of the wiped film type molecular distillation device, setting the distillation temperature to be 160 ℃, preheating heating oil, starting the heating oil circulating pump, starting a molecular distillation device wiped film device rotor, and adjusting to the specified rotating speed of 10 r/min; and opening the vacuum pump, and adjusting the vacuum degree of the vacuum pump to be-0.07 MPa when the pressure is not reduced any more.

[4] The anti-clockwise turning sample injector valve adjusts the sample injection speed, and in the running process of the equipment, the amount of the liquid inlet quantity can be controlled by the sample injector valve, a liquid level measuring device is arranged in the feed chute, and the liquid is automatically supplemented when the liquid level is lower than 30% of the liquid level in the feed chute.

A wiped film type molecular distillation device for removing odor substances in prickly ash seed oil is an improvement on the cloth and scraper of the existing wiped film type molecular distillation device, as shown in figures 1 and 2, the wiped film type molecular distillation device comprises a cylinder body 1 provided with a jacket, a heating oil circulating system 2 is connected on the jacket of the cylinder body 1, a condensing pipe 3 is arranged in the cylinder body 1, a water cooling circulating system 4 is connected on the condensing pipe 3, a vacuumizing device 5 is arranged on the cylinder body 1, a heavy component collecting port is arranged at the bottom of the cylinder body 1 and is connected with a heavy component collecting tank 10, a light component collecting tank 11 is sleeved at the bottom of the condensing pipe 3, a light component discharging port is arranged on the light component collecting tank 11 and is connected with a light component collecting tank 12, a motor 6 is arranged on the cylinder body 1, a component disc 7 is arranged in the cylinder body 1, and the output shaft of the motor 6 is connected with the circle center of the component disc 7, one or two gaps 8 are arranged on the material distribution disc 7, the bottom surface of the material distribution disc 7 at the gap 8 is in contact with the inner wall of the barrel 1, the material distribution disc 7 is connected with a scraper 9, a scraper blade of the scraper 9 is in clearance fit with the inner wall of the barrel 1, the scraper 9 is composed of 2-4 sections of scraper blades 91, the 2-4 sections of scraper blades 91 are arranged in a staggered mode from top to bottom step by step, two adjacent scraper blades 91 are connected through a connecting plate 92, in order to ensure the running stability of the scraper blades, a rotary disc 13 is sleeved outside the light component collecting tank 11, and the scraper blade 91 at the lowest position is connected with the rotary disc 13. The principle that the 2-4 segments of the scraping blades 91 are arranged in a staggered way from top to bottom is that the position of the notch 8 is taken as a starting position, and the scraping blades 91 which are higher pass through the starting position more quickly: the smaller the clearance between the 2-4 sections of the scraping blades 91 and the inner wall of the cylinder body 1 from top to bottom. For the convenient maintenance doctor-bar 91, doctor-bar 91 includes the strip mounting panel of scraping of stereoplasm and the strip of scraping of flexible material, scrapes the strip mounting panel and scrapes the strip and adopts the mortise grafting mode to connect.

During the use, the prickly ash seed oil that falls into the preliminary treatment on the branch charging tray 7 is got rid of to the inner wall of barrel 1 by breach 8 on the branch charging tray 7 under the effect of centrifugal force, then is paintd on the inner tube wall of barrel 1 by the topmost doctor-bar 91 on scraper blade 9, and under the effect of second section doctor-bar, is paintd once more again under the effect of dead weight and liquid converge gradually downwards, and in-process liquid film that goes down in proper order is more and more thin and then accomplishes the molecular distillation, gets rid of the foul substance from the light phase, obtains finished product prickly ash seed oil from the heavy phase.

Claims

1. A method for removing odor substances in pricklyash seed oil is characterized by comprising the following steps: distilling the pretreated pricklyash seed oil by using molecular distillation equipment, removing odor substances from the light phase, and obtaining finished pricklyash seed oil from the heavy phase.

2. The method for removing the odor substances in the prickly ash seed oil according to claim 1, which is characterized in that: the pretreated pricklyash seed oil is obtained by deacidifying and decolorizing crude pricklyash seed oil, and the acid value of the treated pricklyash seed oil is less than 3.0 (KOH)/(mg/g); the crude oil of pepper seeds is prepared by squeezing pepper seeds and extracting by supercritical CO 2.

3. The method for removing the odor substances in the prickly ash seed oil according to claim 1, which is characterized in that: the distillation equipment is a wiped film type molecular distillation device, the distillation temperature of the wiped film type molecular distillation device is set to be 160-.

4. The utility model provides a scrape diaphragm type molecular distillation plant for getting rid of stink material in prickly ash seed oil, it is including barrel (1) that is equipped with the clamp cover, be connected with heating oil circulation system (2) on the clamp cover of barrel (1), be equipped with condenser pipe (3) in barrel (1), be connected with water cooling circulation system (4) on condenser pipe (3), be equipped with evacuating device (5) on barrel (1), be equipped with heavy ends collection mouth in the bottom of barrel (1), heavy ends collection mouth is connected with heavy ends collection tank (10), light ends collecting vat (11) have been cup jointed in the bottom of condenser pipe (3), be equipped with the light ends discharge gate on light ends collecting vat (11), the light ends discharge gate is connected with light ends collection tank (12), its characterized in that: the automatic feeding device is characterized in that a motor (6) is arranged on the barrel body (1), a material distribution disc (7) is arranged in the barrel body (1), an output shaft of the motor (6) is connected with the circle center of the material distribution disc (7), one or two notches (8) are arranged on the material distribution disc (7), the bottom surface of the material distribution disc (7) at the notches (8) is in contact with the inner wall of the barrel body (1), a scraper (9) is connected onto the material distribution disc (7), and a scraper of the scraper (9) is in clearance fit with the inner wall of the barrel body (1).

5. The wiped film type molecular distillation device for removing odor substances in prickly ash seed oil according to claim 4, wherein: the scraping plate (9) is composed of 2-4 sections of scraping plates (91), the 2-4 sections of scraping plates (91) are arranged in a staggered mode from top to bottom, and every two adjacent scraping plates (91) are connected through a connecting plate (92).

6. The wiped film type molecular distillation device for removing odor substances in prickly ash seed oil according to claim 5, wherein: a rotating disc (13) is sleeved outside the light component collecting tank (11), and a scraping blade (91) at the lowest part is connected with the rotating disc (13).

7. The wiped film type molecular distillation device for removing odor substances in prickly ash seed oil according to claim 5 or 6, wherein: the 2-4 sections of the scraping blades (91) are arranged in a staggered mode from top to bottom in a step-by-step mode, the position of the notch (8) is used as a starting position, and the scraping blades (91) which are higher pass the starting position faster.

8. The wiped film type molecular distillation device for removing odor substances in prickly ash seed oil according to claim 7, wherein: the clearance between the 2-4 sections of the scraping blades (91) and the inner wall of the cylinder body (1) is smaller from top to bottom.

9. The wiped film type molecular distillation device for removing odor substances in prickly ash seed oil according to claim 8, wherein: the scraping blade (91) comprises a hard scraping strip mounting plate and a scraping strip made of flexible materials, and the scraping strip mounting plate and the scraping strip are connected in a tenon inserting mode.