Automatic extraction separation apparatus and method for boron trifluoride in alpha-olefin polymerization products

Abstract

The application discloses an automatic extraction and separation device and method for trifluoroboron in alpha-olefin polymerization products. The automatic extraction and separation device comprises an extraction unit, an image acquisition unit, a control unit, a sample storage (5), an extraction liquid storage (6), a lower layer supernatant collector (7), an upper layer supernatant collector (8) and a waste liquid collector (9); the sample storage (5) stores alpha-olefin polymerization products to be extracted; and the extraction liquid storage (6) stores an extraction liquid prepared by mixing alcohol and inorganic alkali. The automatic extraction and separation device uses the extraction liquid prepared by mixing alcohol and inorganic alkali to automatically extract and separate trifluoroboron in alpha-olefin polymerization products.

Description

Technical Field

[0001] This invention relates to the field of chemical separation technology, specifically to an automated extraction and separation device and method for boron trifluoride in α-olefin polymerization products. Background Technology

[0002] Alpha-olefin polymerization is a major method for producing lubricating oil base oils, and boron trifluoride (BF3) catalyst is one of the commonly used catalysts in this process. During production, a small amount of BF3 from the catalyst often remains in the base oil and intermediate products in gaseous-liquid form due to fluctuations in the production process. BF3 that enters the product reacts with moisture in the air to form a strong acid, corroding production equipment and components, and affecting the continuous and stable operation of the unit. Furthermore, excessively high fluorine content directly affects subsequent hydrogenation processes, as well as catalyst performance and lifespan. Excessive fluorine content in the base oil product affects product quality and can corrode engines and other equipment and components during use, posing threats to equipment, personnel health, and environmental protection.

[0003] Therefore, it is necessary to monitor the fluoride content in lubricating oil base oil at all times. Since fluorides are corrosive, burning fluoride-containing lubricating oil base oil at high temperatures can severely corrode the combustion pipe. Therefore, using an extraction method to extract the fluoride and detecting the fluoride content in the extract can achieve safe and efficient detection of the fluoride content in the base oil.

[0004] Extraction is a commonly used operation method in laboratory analysis. Traditional extraction methods rely on manual weighing of liquid volume, adding liquid to the separatory funnel, manual shaking and oscillation, and separation and collection of the upper and lower liquids. This is inefficient, increases labor intensity, and raises labor costs. During the extraction process, laboratory personnel come into contact with harmful volatile solvents, posing a threat to their health. Shaking extraction, settling time, and collection of the upper and lower liquids all require manual control and setting, resulting in a very low degree of automation and susceptibility to human interference.

[0005] With the continuous development and upgrading of analytical technologies, analytical instruments are gradually moving towards higher levels of automation and intelligence to improve operational convenience and analytical efficiency, greatly promoting the widespread application of analytical instruments. The development of image processing technology has driven the emergence and development of image recognition technology, which has gradually become an important component of the field of artificial intelligence. Currently, image recognition is widely used in the petrochemical industry, such as oil and gas exploration, coal seam identification, and non-destructive testing. The development of science and technology has also placed increasingly higher demands on modern instruments and equipment. People not only require accurate and reliable sample separation and extraction, but also more timely, efficient, and automated processing and analytical experiences. In today's laboratories, routine operations such as extraction occupy most of the laboratory staff's time. Reducing the time spent by laboratory analysts on these repetitive operations would undoubtedly greatly improve experimental efficiency. The integration of image recognition technology with instruments and equipment can greatly improve the automation level of instruments and equipment and increase production efficiency.

[0006] CN 207042499U discloses an automatic oscillating extraction separatory funnel, including a body, a rotating shaft, a motor, and control buttons. The rotating shaft is mounted on the body, and a retainer is mounted on the shaft. Clamping plates are mounted on both sides of the retainer, and the separatory funnel is positioned between the retainer and the clamping plates. The rotating shaft drives the separatory funnel to tumble up and down, replacing manual oscillation. A control box and display screen are located on the side of the body, allowing for speed adjustment and timer settings. While this technology uses a motor to drive the rotating shaft and tumble the separatory funnel to replace manual oscillation, manual operation is still required when adding liquid to the separatory funnel. The liquid is easily contaminated during weighing and transfer, increasing workload. After the liquid settles and separates into layers, the operator needs to manually collect the upper layer, lower layer, and waste liquid (mixture at the separation point). When the sample is valuable and it is necessary to recover as much of the upper or lower layer liquid as possible, the operator needs to be skilled in operating the separatory funnel to avoid over-collection or waste of liquid due to errors. This requires a certain level of experience from the operator, has a low degree of automation, and affects work efficiency.

[0007] CN 204649511U discloses a fully automatic extraction device with a distance sensor, including a first liquid container, a second liquid container, an inlet valve, a drain valve, a non-contact distance sensor, a reflective photoelectric sensor, a nitrogen source, a vacuum pump, an extraction disc, a gas pipeline, a first liquid pipeline, a second liquid pipeline, an extraction vacuum pipeline, and a control module. The non-contact distance sensor is an ultrasonic sensor, placed above the extraction disc, while the reflective photoelectric sensor is placed on one side of the extraction disc. First, the type of extraction disc is determined based on the reflective photoelectric sensor, thereby determining the volume of the extraction disc. Liquid is drawn from the first and second liquid pipelines into the extraction disc. The distance to the liquid surface is detected by the ultrasonic sensor to determine the liquid volume. When the liquid volume reaches a set value, the solenoid valve is closed, and during drainage, negative pressure forces the liquid in the extraction disc into a collection container. This technology relates to a fully automatic extraction device with a distance sensor, which uses an ultrasonic sensor to detect the distance to the liquid surface and determine the liquid volume, thereby controlling the intake and discharge of liquid in the extraction disc. Because ultrasonic sensors are highly sensitive to temperature changes of 5-10°C or higher, which can affect sensing accuracy; ultrasonic waves are difficult to accurately reflect from small objects, thus significantly impacting the accuracy of liquid volume estimation when the liquid in the extraction pan is low; and ultrasonic waves are highly sensitive to nearby equipment and the environment, as vibrations from nearby instruments or the environment can affect the accuracy of distance measurements. Furthermore, ultrasonic waves can only determine the liquid level in the extraction pan, but cannot detect the degree of separation at the phase interface after stratification. This is especially problematic for extracts containing impurities at the interface, making it difficult to accurately set the discharge volume of the lower liquid and the mixed waste liquid at the phase interface, which can easily lead to sample loss or contamination of the extract. Summary of the Invention

[0008] The purpose of this invention is to provide an automated extraction and separation device and method for boron trifluoride in α-olefin polymerization products.

[0009] To achieve the above objectives, the present invention adopts the following technical solution:

[0010] The present invention provides an automatic extraction and separation device for boron trifluoride in α-olefin polymerization products, wherein the automatic extraction and separation device includes: an extraction unit, an image acquisition unit, a control unit, a sample storage unit, an extraction liquid storage unit, a lower clear liquid collector, an upper clear liquid collector, and a waste liquid collector;

[0011] The sample storage unit stores the α-olefin polymerization product to be extracted, and the extraction solution storage unit stores an extraction solution prepared from an alcohol and an inorganic base; the alcohol and the inorganic base cannot react with each other;

[0012] The sample storage and extraction liquid storage are connected to the inlet of the extraction unit via pipelines; the outlet of the extraction unit is connected to the lower clear liquid collector, the upper clear liquid collector, and the waste liquid collector, respectively; the extraction unit is within the image acquisition range of the image acquisition unit;

[0013] The control unit controls the sample storage and extraction liquid storage to input preset volumes of the α-olefin polymerization product to be extracted and the extraction liquid to the extraction unit, respectively. It controls the extraction unit to perform oscillating mixing for a preset time and static stratification for a preset time. It also controls the image acquisition unit to acquire images of the extraction unit and identify the position of the phase interface. Based on the identified phase interface position, it controls the discharge of the extraction unit.

[0014] The drainage process includes: draining a predetermined volume of lower layer liquid into the lower clear liquid collector, draining the remaining lower layer liquid and the mixture at the phase interface into the waste liquid collector, and draining a predetermined volume of upper layer liquid into the upper clear liquid collector.

[0015] During the drainage process, if there is still residual upper liquid after the extraction unit has discharged a preset volume of upper liquid, it is discharged into the waste liquid collector.

[0016] According to the automatic extraction and separation apparatus of the present invention, preferably, the automatic extraction and separation apparatus further includes an input unit for inputting the preset volume and preset duration to the control unit. The input unit may be a keyboard, an app, or other medium, and the present invention does not limit this to such a medium.

[0017] According to the automatic extraction and separation apparatus of the present invention, preferably, the automatic extraction and separation apparatus further includes a display unit for displaying the input signals and status information of the control unit. The status information includes, for example, the progress of the control process and information acquired by the image acquisition unit. The display unit can be a screen or other medium with display function; the present invention does not limit this. Furthermore, the input unit and the display unit can be integrated, for example, integrated into an operation panel that can both input and display; or, for example, into an app program that can run on any smart terminal and can simultaneously input and display. The present invention does not limit this.

[0018] Furthermore, the device of the present invention may not include the input unit and the display unit. The control unit can be pre-programmed and can be run directly later. In addition, the control unit can also be pre-programmed with different programs so that the operator can select a more suitable pre-program according to the specific amount of liquid to be extracted.

[0019] According to the automatic extraction and separation device of the present invention, preferably, the extraction unit includes an extraction container and a shaking rack, wherein the extraction container is mounted on the shaking rack; one or more extraction containers may be installed as needed, and the extraction container may be any container capable of extraction, such as a separatory funnel or an extraction tube.

[0020] According to the automatic extraction and separation apparatus of the present invention, preferably, the sample storage and the extraction liquid storage are connected to the top inlet of the extraction container via a first suction line and a second suction line, respectively; both the first and second suction lines are equipped with a pump and a solenoid valve. More preferably, a rigid needle is installed at the starting end of the first and second suction lines for puncturing and sampling volatile samples. The starting end refers to one end located in the sample storage and the extraction liquid storage.

[0021] According to the automatic extraction and separation device of the present invention, preferably, a solenoid valve is provided at the bottom outlet of the extraction container, and the bottom outlet of the extraction container is connected to the lower clear liquid collector, the upper clear liquid collector, and the waste liquid collector respectively through a four-way valve, and an electromagnetic flow meter is provided on each of the connecting pipelines.

[0022] According to the automatic extraction and separation apparatus of the present invention, preferably, the image acquisition unit includes a slide bar and an image acquisition component that is slidably mounted on the slide bar; the slide bar is vertically parallel to the extraction container. The image acquisition component is, for example, a conventional camera or an infrared camera.

[0023] During operation, the image acquisition unit (e.g., a camera) can slide up and down to track the phase interface in the extraction container. After the phase separation is completed, the liquid is drained. During the draining process, the descent of the phase interface is tracked. After a preset volume of the lower layer liquid is discharged, the draining process switches to the waste liquid collector. After the mixture of the phase interface is completely discharged from the bottom outlet of the extraction container (e.g., the lower diameter of the separatory funnel), the draining process switches to the clear liquid collector.

[0024] In the automatic extraction and separation device according to the present invention, preferably, the distance between the image acquisition component and the extraction container is 10~100 cm.

[0025] According to the automatic extraction and separation device of the present invention, preferably, a liquid intake port is provided above the upper clear liquid (oil) collector and connected to the feed port of the extraction unit; the connection can be a switchable connection or a fixed connection, and the present invention does not limit the specific connection method here.

[0026] When multiple extractions are required, the supernatant collected in the supernatant collector can be transferred to the extraction container for repeated extraction. Specifically, the transfer can be achieved by directly inserting the first suction line into the supernatant collector through the suction port, or by directly connecting the suction port to the top inlet of the extraction container. A solenoid valve can also be installed on the connecting line, allowing the control system to directly control the repeated extraction. Both transfer methods avoid liquid contamination or loss caused by transferring liquid during multiple extractions.

[0027] In the device of the present invention, each connecting pipe is preferably made of PU hose.

[0028] According to the automatic extraction and separation apparatus of the present invention, preferably, the alcohol in the extract is ethylene glycol. More preferably, the alkali in the extract is sodium carbonate and / or potassium carbonate. Even more preferably, the mass percentage of sodium carbonate and / or potassium carbonate in the extract is 0.1% to 4% (preferably 0.5% to 4%).

[0029] Adding an inorganic base to the alcohol extract helps neutralize the acidic substance boron trifluoride, reducing the amount of alcohol extract needed and improving extraction efficiency. Methanol and ethanol react chemically with inorganic bases such as sodium carbonate, while ethylene glycol does not react with sodium carbonate or potassium carbonate. Furthermore, since ethylene glycol reacts with sodium hydroxide, sodium hydroxide is not used as the base; and sodium carbonate is readily available, more common, and cheaper than potassium carbonate, making the more readily available sodium carbonate a better choice.

[0030] According to the automatic extraction and separation apparatus of the present invention, preferably, the volume ratio of the extract to the α-olefin polymerization product to be extracted is 1:(1~50); more preferably, it is 1:(1~2.5).

[0031] According to the automatic extraction and separation apparatus of the present invention, preferably, during the drainage process, the preset volume of the lower layer liquid discharged into the lower clear liquid collector is not greater than the input volume of the extractant; the preset volume of the upper layer liquid discharged into the upper clear liquid collector is not greater than the input volume of the α-olefin polymerization product to be extracted. The specific preset volume can be set according to experimental needs, etc., and the present invention does not limit this.

[0032] Another aspect of the present invention provides an automated extraction and separation method for boron trifluoride in α-olefin polymerization products, which is performed using any of the above-mentioned automated extraction and separation devices.

[0033] According to the automated extraction and separation method of the present invention, preferably, the automated extraction and separation method includes the following processes:

[0034] A predetermined volume of the α-olefin polymerization product (containing BF3) to be extracted and the extract prepared by the alcohol and inorganic base are input into the extraction unit, and the mixture is subjected to shaking and mixing for a predetermined time and standing for a predetermined time to separate into layers, and then the liquid is drained; the alcohol and the inorganic base cannot react with each other.

[0035] According to the automatic extraction and separation method of the present invention, preferably, the alcohol in the extract is ethylene glycol. More preferably, the inorganic base in the extract is sodium carbonate and / or potassium carbonate, and the mass percentage of sodium carbonate and / or potassium carbonate in the extract is 0.1% to 4%; more preferably, it is 0.5% to 4%.

[0036] According to the automatic extraction and separation method of the present invention, preferably, the volume ratio of the extract to the α-olefin polymerization product to be extracted is 1:(1~50); more preferably, it is 1:(1~2.5).

[0037] The preset duration of the oscillation mixing, the oscillation frequency, and the preset duration of the settling and stratification can be adjusted according to the actual usage effect. This invention does not limit these settings; only preferred ranges are listed here. Preferably, the preset duration of the oscillation mixing is 10-60 min; more preferably, 10-20 min. Preferably, the oscillation frequency of the oscillation mixing is 100-400 rpm; more preferably, 150-260 rpm. Preferably, the preset duration of the settling and stratification is 2-10 h; more preferably, 5-10 h.

[0038] According to the automated extraction and separation method of the present invention, preferably, the draining specifically includes:

[0039] The control unit controls the discharge of a preset volume of lower layer liquid into the lower clear liquid collector, and then controls the discharge of the remaining lower layer liquid and the mixture at the phase interface into the waste liquid collector. Once the image acquisition unit detects that the mixture at the phase interface has been completely discharged from the extraction unit, it controls the discharge of a preset volume of upper layer liquid into the upper clear liquid collector. More preferably, if there is still remaining upper layer liquid after the preset volume of upper layer liquid has been discharged from the extraction unit, it is discharged into the waste liquid collector.

[0040] In a preferred embodiment, the switching of drainage during the drainage process is achieved by switching a four-way valve.

[0041] According to the automatic extraction and separation method of the present invention, preferably, when multiple extractions are required, the supernatant (oil) collected in the supernatant collector is transferred to the extraction container of the extraction unit for repeated extraction.

[0042] The beneficial effects of this invention include:

[0043] 1) By extracting BF3 remaining in the α-olefin polymerization product, corrosion caused by the reaction equipment and subsequent applications is avoided, as is corrosion of the quartz combustion tube when detecting fluorine content during high-temperature cracking of oil.

[0044] 2) Adding sodium carbonate and / or potassium carbonate to alcohol helps neutralize the acidic substance boron trifluoride, which can reduce the amount of alcohol reagent used and improve extraction efficiency.

[0045] 3) An image acquisition unit is set up to acquire and identify the changes in the liquid level and phase interface position throughout the extraction process. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to the upper clear liquid collector and discharges a preset volume of upper liquid into the upper clear liquid collector. The image recognition technology is used for real-time monitoring and detection, which is not affected by the height and position of the liquid level in the separatory funnel, thus improving the automation of the extraction.

[0046] 4) The four-way valve is designed to accurately switch between collecting the lower clear liquid, waste liquid and upper clear liquid based on real-time information from image recognition. There is no need for manual operation of the separatory funnel switch, saving manpower, reducing human operation error, and avoiding sample loss and extraction liquid contamination caused by human operation in complex situations such as poor two-phase separation effect or impurities at the phase interface.

[0047] 5) The system has a preset liquid aspiration volume. The aspiration tube can be directly placed into the sample storage to automatically aspirate the sample. When extracting again, the aspiration tube can be directly inserted into the liquid collector. There is no need to weigh the sample and transfer it to the separatory funnel, which simplifies the operation and avoids the sample being contaminated during weighing and transfer. Attached Figure Description

[0048] Figure 1 This is a schematic diagram of an automatic extraction and separation device for boron trifluoride in α-olefin polymerization products according to a preferred embodiment of the present invention.

[0049] Figure 2 This is a schematic diagram showing the positions of the image acquisition unit and the separating funnel in a preferred embodiment of the present invention.

[0050] Explanation of reference numerals in the attached figures:

[0051] 1. Extraction container;

[0052] 2. Vibration frame;

[0053] 3. First solenoid valve;

[0054] 4. Second solenoid valve;

[0055] 5. Sample storage;

[0056] 6. Extraction solution storage;

[0057] 7. Lower layer clear liquid collector;

[0058] 8. Supernatant collector;

[0059] 9. Waste liquid collector;

[0060] 10. Third solenoid valve;

[0061] 11. Four-way valve;

[0062] 12. Image acquisition component;

[0063] 13. Slide bar. Detailed Implementation

[0064] To more clearly illustrate the present invention, the following description, in conjunction with preferred embodiments, further clarifies the invention. Those skilled in the art should understand that the specific descriptions below are illustrative rather than restrictive, and should not be construed as limiting the scope of protection of the present invention.

[0065] like Figure 1 As shown, the present invention provides an automatic extraction and separation device for boron trifluoride in α-olefin polymerization products, comprising: an extraction unit, an image acquisition unit, a control unit, a sample storage unit 5, an extraction liquid storage unit 6, a lower clear liquid collector 7, an upper clear liquid collector 8, and a waste liquid collector 9.

[0066] The sample storage 5 stores the α-olefin polymerization product to be extracted, and the extraction liquid storage 6 stores an extraction liquid prepared from an alcohol and an inorganic base; the alcohol and the inorganic base cannot react with each other; preferably, the extraction liquid is prepared from ethylene glycol and sodium carbonate and / or potassium carbonate, more preferably, the extraction liquid is prepared from ethylene glycol and sodium carbonate;

[0067] The sample storage 5 and the extraction liquid storage 6 are connected to the inlet of the extraction unit via pipelines; the outlet of the extraction unit is connected to the lower clear liquid collector 7, the upper clear liquid collector 8, and the waste liquid collector 9, respectively; the extraction unit is within the image acquisition range of the image acquisition unit.

[0068] The control unit controls the sample storage 5 and the extraction liquid storage 6 to input a preset volume of the α-olefin polymerization product to be extracted and the extraction liquid to the extraction unit, respectively. It controls the extraction unit to perform a preset duration of shaking mixing and a preset duration of static stratification, and controls the image acquisition unit to acquire images of the extraction unit and identify the position of the phase interface. Based on the identified phase interface position, it controls the discharge of the extraction unit.

[0069] The drainage process includes: draining a preset volume of lower layer liquid into the lower clear liquid collector 7; draining the remaining lower layer liquid and the mixture at the phase interface into the waste liquid collector 9; and draining a preset volume of upper layer liquid into the upper clear liquid collector 8. If there is still remaining upper layer liquid after the preset volume of upper layer liquid has been drained from the extraction unit, it is drained into the waste liquid collector 9. Image recognition technology is used for real-time monitoring and detection during the drainage process. When the image acquisition unit detects that the mixture at the phase interface has been completely drained from the extraction unit, it switches to the upper clear liquid collector to collect the preset volume of upper layer liquid.

[0070] The automatic extraction and separation device of the present invention may further include an input unit and / or a display unit. The input unit is used to input the preset volumes and preset durations to the control unit, and can be a keyboard, an app, or other medium, which is not limited in the present invention. The display unit is used to display the input signals and status information of the control unit, including, for example, the progress of the control process and information acquired by the image acquisition unit. The display unit can be a screen or other medium with display function, which is not limited in the present invention. Furthermore, the input unit and the display unit can be integrated, for example, integrated into an operation panel that can both input and display; or, for example, into an app program that can run on any smart terminal and can simultaneously input and display. This is not limited in the present invention. Furthermore, the device of the present invention may not include the input unit and the display unit; the control unit can be pre-programmed and run directly later; in addition, the control unit can be pre-programmed with different programs so that the operator can select a more suitable pre-set program according to the specific amount of liquid to be extracted.

[0071] exist Figure 1 In the preferred embodiment shown, the extraction unit includes an extraction container 1 and a shaking rack 2, with the extraction container 1 mounted on the shaking rack 2. One or more extraction containers 1 can be installed as needed, and the extraction container 1 can specifically be any container capable of extraction, such as... Figure 1 In addition to the separatory funnel, it can also be an extraction tube, etc.

[0072] exist Figure 1In the preferred embodiment shown, the sample storage 5 and the extraction liquid storage 6 are respectively connected to the top inlet of the extraction container 1 via a first suction line and a second suction line; each of the first and second suction lines is equipped with a pump for drawing liquid, and a first solenoid valve 3 and a second solenoid valve 4 are respectively provided for control by the control unit; the opening of the pump is also controlled by the control unit. More preferably, a rigid needle is installed at the starting end of the first and second suction lines for puncturing and sampling volatile samples; details are further elaborated on the following pages. The starting end refers to one end located in the sample storage 5 and the extraction liquid storage 6.

[0073] exist Figure 1 In the preferred embodiment shown, a third solenoid valve 10 is preferably provided at the bottom outlet of the extraction container 1, and the bottom outlet of the extraction container 1 is connected to the lower clear liquid collector 7, the upper clear liquid collector 8, and the waste liquid collector 9 respectively through a four-way valve 11, and an electromagnetic flow meter is provided on each of the connecting pipelines.

[0074] like Figure 2 As shown, in a preferred embodiment, the image acquisition unit includes a slide bar 13 and an image acquisition component 12 that can be slidably mounted on the slide bar 13; the slide bar 13 is vertically parallel to the extraction container 1. The image acquisition component 12 is, for example, a common camera or an infrared camera.

[0075] During operation, the image acquisition unit 12 (e.g., a camera) can slide up and down to track the phase interface in the extraction container 1. After the phase separation is completed, the liquid is drained. During the draining process, the descent of the phase interface is tracked. After a preset volume of lower liquid is discharged, the draining process switches to the waste liquid collector 9. After the mixture of phase interface is completely discharged from the bottom outlet of the extraction container 1 (e.g., the lower diameter of the separating funnel), the draining process switches to the upper clear liquid collector 8.

[0076] More preferably, the distance between the image acquisition component 12 and the extraction container 1 is 10~100 cm.

[0077] In another preferred embodiment of the present invention, a liquid intake port is preferably provided above the upper clear liquid collector 8, which is connected to the feed inlet of the extraction unit to complete multiple extractions. The connection can be a switchable connection or a fixed connection, and the present invention does not limit the specific connection method here.

[0078] When multiple extractions are required, the supernatant (oil) collected in the supernatant collector 8 can be transferred to the extraction container 1 for repeated extraction. Specifically, the transfer can be achieved by directly inserting the first suction line into the supernatant collector 8 through the suction port, or by directly connecting the suction port to the top inlet of the extraction container 1. A solenoid valve can also be installed on the connecting line to directly control the repeated extraction via a control system. Both transfer methods avoid liquid contamination or loss caused by transferring liquid during multiple extractions.

[0079] In the above devices, PU hoses are preferably used for all connecting pipes.

[0080] Regarding the extractant: the alcohol is preferably ethylene glycol, and the inorganic base is preferably sodium carbonate and / or potassium carbonate, with the mass percentage of sodium carbonate and / or potassium carbonate in the extractant being 0.1% to 4%, more preferably 0.5% to 4%. Adding sodium carbonate and / or potassium carbonate to the alcohol extractant helps neutralize the acidic substance boron trifluoride, reducing the amount of alcohol extractant used and improving extraction efficiency. Methanol and ethanol react chemically with inorganic bases such as sodium carbonate, while ethylene glycol does not react with sodium carbonate or potassium carbonate. Furthermore, since ethylene glycol reacts with sodium hydroxide, sodium hydroxide is not used as the base; and since sodium carbonate is readily available, more common, and cheaper than potassium carbonate, the more common sodium carbonate is preferred.

[0081] The volume ratio of the extract to the α-olefin polymerization product to be extracted is preferably 1:(1~50); more preferably 1:(1~2.5).

[0082] During the drainage process, the preset volume of the lower layer liquid discharged into the lower clear liquid collector 7 is not greater than the input volume of the extract; the preset volume of the upper layer liquid discharged into the upper clear liquid collector 8 is not greater than the input volume of the α-olefin polymerization product to be extracted. The specific preset volume can be set according to experimental needs, etc., and this invention does not limit it.

[0083] The automated extraction and separation method for boron trifluoride in α-olefin polymerization products using any of the above automated extraction and separation devices includes the following steps:

[0084] The α-olefin polymerization product (containing BF3) to be extracted and the extract solution prepared by alcohol and inorganic base are fed into the extraction unit, and the mixture is shaken and mixed for a preset time and allowed to stand for a preset time to separate into layers, and then the liquid is drained.

[0085] The preset duration of the oscillation mixing is preferably 10-60 min, more preferably 10-20 min. The oscillation frequency of the oscillation mixing is preferably 100-400 rpm, more preferably 150-260 rpm. The preset duration of the settling and stratification is preferably 2-10 h, more preferably 5-10 h.

[0086] The drainage specifically includes:

[0087] The control unit controls the discharge of a preset volume of lower liquid into the lower clear liquid collector 7, and then controls the discharge of the remaining lower liquid and the mixture at the phase interface into the waste liquid collector 9. After the image acquisition unit detects that the mixture at the phase interface has been completely discharged from the extraction unit, it controls the discharge of a preset volume of upper liquid into the upper clear liquid collector 8.

[0088] In a preferred embodiment, using Figure 1 and Figure 2 The automated extraction and separation method for boron trifluoride in α-olefin polymerization products, as shown in the automated extraction and separation apparatus, includes the following steps:

[0089] Place the α-olefin polymerization product in sample storage 5, and place an ethylene glycol extract with a mass fraction of 0.1% to 4% sodium carbonate and / or potassium carbonate in extract storage 6. Set the extractant-to-oil ratio of ethylene glycol extract to lubricating oil base oil to 1:1 to 1:50, set the extraction oscillation time to 10 to 60 min, the settling time to separate layers to 2 to 10 h, and the extraction oscillation frequency to 100 to 400 rpm. The preset collection volumes of the upper and lower layers should not exceed the preset volumes of the sample to be extracted and the extractant, respectively. Place the hard needles at the beginning of the first and second suction lines into the extractant and start the equipment. Start the pumps on the first and second suction lines, and aspirate the preset volume of liquid into the separatory funnel. After aspiration is complete... The shaking rack 2 is started to shake and extract the liquid in the separating funnel for a preset time. After shaking stops and the liquid is allowed to settle and separate, the liquid discharge program is started. The image acquisition unit acquires the image of the separating funnel and identifies the phase interface position. The four-way valve 11 is switched to the lower clear liquid collector 7. After the lower clear liquid is discharged into the lower clear liquid collector 7 according to the preset volume, the four-way valve 11 is switched to the waste liquid collector 9. The remaining lower clear liquid and the mixed liquid at the phase interface are discharged into the waste liquid collector 9. When the image acquisition unit identifies that the mixed liquid at the phase interface has been completely discharged from the separating funnel, the four-way valve 11 is switched to the upper clear liquid collector 8. The preset volume of upper clear liquid is discharged into the upper clear liquid collector 8. If there is any remaining upper clear liquid, the remaining upper clear liquid is placed into the waste liquid collector 9.

[0090] The following are some specific application examples to further illustrate this point. Unless otherwise specified, the reagents and compounds involved are all commercially available.

[0091] Evaluation and analysis methods: Fluorine content in α-olefin polymerization products was determined using a 940MCIC combustion furnace ion chromatograph.

[0092] Application Example 1

[0093] The α-olefin polymerization product to be extracted is placed in sample storage 5. A sodium carbonate solution with a mass fraction of 0.1% ethylene glycol is added to extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes are placed in sample storage 5 and extraction solution storage 6, respectively. The preset amounts of sample to be extracted, 8 mL of extraction solution, 10 mL of upper clear liquid (oil), and 5 mL of lower clear liquid (alcohol) are set on the operation panel. The shaking frequency is 150 rpm, the shaking time is 10 min, and the mixture is allowed to stand for 5 h to separate. The device is then started, and the first solenoid valve 3 and the second solenoid valve 4 are opened. Liquid is drawn into the separatory funnel according to the preset volume. After the liquid is drawn, the extraction is complete. The shaking rack 2 is started to shake and extract the liquid in the separatory funnel for a preset time of 10 minutes. After shaking stops and the mixture is allowed to stand for 5 hours to separate into layers, the third solenoid valve 10 and the image acquisition component 12 at the outlet of the separatory funnel are opened, and the four-way valve 11 is switched to outlet C. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition component 12 slides down along the slide bar 13 to monitor and identify the phase interface and liquid surface position in the separatory funnel, and acquires the image of the separatory funnel and identifies the phase interface position. When the electromagnetic flowmeter detects that the flow rate reaches the preset 5 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit recognizes that the mixed liquid at the phase interface has been completely discharged from the separating funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 10 mL, the four-way valve switches to outlet a, and the remaining liquid is discharged into the waste liquid collector 9, completing one extraction. If it is necessary to extract the liquid again after extraction, the first and second suction lines can be directly inserted into their respective collectors to suction the liquid.

[0094] The fluorine content in the α-olefin polymerization product before extraction was 83.3 mg / L, and the fluorine content after extraction was 13.5 mg / L.

[0095] Application Example 2

[0096] The α-olefin polymerization product to be extracted is placed in sample storage 5. A sodium carbonate solution with a mass fraction of 1.5% in ethylene glycol is added to extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes are placed in sample storage 5 and extraction solution storage 6, respectively. The preset volume of sample to be extracted is 75 mL, the volume of extractant is 30 mL, the volume of upper clear liquid (oil) is 45 mL, and the volume of lower clear liquid (ethylene glycol) is 25 mL. The shaking frequency is 150 rpm, the shaking time is 10 min, and the mixture is allowed to stand for 5 h to separate. The device is then started, the first solenoid valve 3 and the second solenoid valve 4 are opened, and the preset volume of liquid is drawn into the separatory funnel. After the liquid is drawn, the extraction is completed. The shaking rack 2 is activated to shake and extract the liquid in the separatory funnel for the preset time. Shaking stops, and the mixture is allowed to stand for 5 hours to separate. After separation, the third solenoid valve 10 and image acquisition unit 12 at the separatory funnel outlet are opened, and the four-way valve 11 is switched to outlet c. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition unit 12 slides downwards along the slide bar 13 to monitor and identify the phase interface and liquid surface positions in the separatory funnel, acquiring images of the separatory funnel and identifying the phase interface positions. When the electromagnetic flowmeter detects that the flow rate reaches the preset volume, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset volume, the four-way valve 11 switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction cycle.

[0097] The fluorine content in the α-olefin polymerization product before extraction was 157.3 mg / L, and the fluorine content after extraction was 5.5 mg / L.

[0098] The extracted liquid was subjected to a second extraction. The rigid needle at the beginning of the first aspiration tube was placed into the supernatant collector 8. The sample volume was again set to 40 mL, the extractant volume to 20 mL, the supernatant volume to 35 mL, and the lower supernatant volume to 15 mL. The shaking frequency was 150 rpm, the shaking time was 10 min, and the mixture was allowed to stand for 5 h before starting the apparatus. The above steps were repeated to obtain the supernatant and lower supernatant after the second extraction. The fluoride content after the second extraction was found to be 0.9 mg / L.

[0099] The extracted liquid was subjected to three extractions. The rigid needle at the beginning of the first aspiration tube was placed into the supernatant collector 8. The sample volume was set to 30 mL, the extractant volume to 15 mL, the supernatant volume to 25 mL, and the lower supernatant volume to 10 mL. The shaking frequency was 150 rpm for 10 min, and the mixture was allowed to stand for 5 h before starting the apparatus. The above steps were repeated to obtain the supernatant and lower supernatant after three extractions. The fluorine content in the α-olefin polymerization product after the three extractions was not detected.

[0100] Application Example 3

[0101] The α-olefin polymerization product was placed in the sample storage 5. A sodium carbonate solution with a mass fraction of 4% ethylene glycol was added to the extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes were placed in the sample storage 5 and the extraction solution storage 6, respectively. The preset sample volume to be extracted was 100 mL, the extractant volume was 40 mL, the upper clear liquid (oil) volume was 35 mL, and the lower clear liquid (ethylene glycol) volume was 35 mL. The shaking frequency was 150 rpm, the shaking time was 10 min, and the mixture was allowed to stand for 5 h. The device was then started, the first solenoid valve 3 and the second solenoid valve 4 were opened, and the preset volume of liquid was drawn into the separatory funnel. After the liquid was drawn, the extraction was completed. The shaking rack 2 is activated to shake and extract the liquid in the separatory funnel for the preset time. Shaking stops, and after 5 hours of settling, the liquid separates into layers. Then, the third solenoid valve 10 and image acquisition unit 12 at the separatory funnel outlet are opened, and the four-way valve 11 switches to outlet c. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition unit 12 slides downwards along the slide bar 13 to monitor and identify the phase interface and liquid surface positions in the separatory funnel, acquiring images of the separatory funnel and identifying the phase interface positions. When the electromagnetic flowmeter detects that the flow rate reaches the preset 35 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 35 mL, the four-way valve switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction cycle.

[0102] The fluorine content in the sample before extraction was 1047.2 mg / L, and the fluorine content in the sample after extraction was 12.7 mg / L.

[0103] The extracted sample was subjected to a second extraction. The rigid needle at the beginning of the first aspiration tube was placed into the supernatant collector 8. The sample volume was set to 30 mL, the extractant volume to 15 mL, the supernatant volume to 25 mL, and the lower supernatant volume to 10 mL. The shaking frequency was 150 rpm, the shaking time was 10 min, and the mixture was allowed to stand for 5 h before starting the apparatus. The above steps were repeated to obtain the supernatant and lower supernatant after the second extraction. The fluorine content in the α-olefin polymerization product after the second extraction was found to be 0.56 mg / L.

[0104] The extracted liquid was subjected to three extractions. The rigid needle at the beginning of the first aspiration tube was placed into the supernatant collector 8. The sample volume was set to 20 mL, the extractant volume to 10 mL, the supernatant volume to 15 mL, and the lower supernatant volume to 8 mL. The shaking frequency was 150 rpm for 10 min, and the mixture was allowed to stand for 5 h before starting the apparatus. The above steps were repeated to obtain the supernatant and lower supernatant after three extractions. The fluorine content in the α-olefin polymerization product after the three extractions was not detected.

[0105] Application Example 4

[0106] The α-olefin polymerization product was placed in the sample storage 5. A sodium carbonate solution with a mass fraction of 4% ethylene glycol was added to the extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes were placed in the sample storage 5 and the extraction solution storage 6, respectively. The preset amounts of sample to be extracted, 20 mL of extractant, 40 mL of upper clear liquid (oil), and 15 mL of lower clear liquid (ethylene glycol) were set on the operation panel. The shaking frequency was 150 rpm, the shaking time was 10 min, and the mixture was allowed to stand for 5 h. The device was then started, and the first solenoid valve 3 and the second solenoid valve 4 were opened. The preset volume of liquid was drawn into the separatory funnel. After the liquid was drawn, the extraction was completed. The shaking rack 2 is activated to shake and extract the liquid in the separatory funnel for the preset time. Shaking stops, and after 5 hours of settling, the liquid separates into layers. Then, the third solenoid valve 10 and image acquisition unit 12 at the separatory funnel outlet are opened, and the four-way valve 11 switches to outlet c. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition unit 12 slides downwards along the slide bar 13 to monitor and identify the phase interface and liquid surface positions in the separatory funnel, acquiring images of the separatory funnel and identifying the phase interface positions. When the electromagnetic flowmeter detects that the flow rate reaches the preset 3 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 40 mL, the four-way valve switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction cycle.

[0107] The fluorine content in the sample before extraction was 83.3 mg / L, and the fluorine content in the sample after extraction was 1.1 mg / L.

[0108] Application Example 5

[0109] The α-olefin polymerization product was placed in the sample storage 5. A sodium carbonate solution with a mass fraction of 4% ethylene glycol was added to the extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes were placed in the sample storage 5 and the extraction solution storage 6, respectively. The preset sample volume to be extracted was 300 mL, the extractant volume was 6 mL, the upper clear liquid (oil) volume was 40 mL, and the lower clear liquid (ethylene glycol) volume was 3 mL. The shaking frequency was 260 rpm, the shaking time was 20 min, and the mixture was allowed to stand for 10 h. The device was then started, the first solenoid valve 3 and the second solenoid valve 4 were opened, and the preset volume of liquid was drawn into the separatory funnel. After the liquid was drawn, the extraction was completed. The shaking rack 2 is activated to shake and extract the liquid in the separatory funnel for the preset time. Shaking stops, and after standing for 10 hours to allow stratification, the third solenoid valve 10 and image acquisition unit 12 at the separatory funnel outlet are opened. The four-way valve 11 is switched to outlet c, and the lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition unit 12 slides downwards along the slide bar 13 to monitor and identify the phase interface and liquid surface position in the separatory funnel, acquiring images of the separatory funnel and identifying the phase interface position. When the electromagnetic flowmeter detects that the flow rate reaches the preset 3 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 40 mL, the four-way valve switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction cycle.

[0110] The fluorine content in the sample before extraction was 157.3 mg / L, and the fluorine content in the sample after extraction was 2.3 mg / L.

[0111] Application Example 6

[0112] The α-olefin polymerization product was placed in the sample storage 5. A 0.1% potassium carbonate ethylene glycol solution was added to the extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes were placed in the sample storage 5 and the extraction solution storage 6, respectively. The preset amounts of sample to be extracted, 20 mL of extractant, 40 mL of upper clear liquid (oil), and 15 mL of lower clear liquid (ethylene glycol) were set on the operation panel. The shaking frequency was 150 rpm, the shaking time was 10 min, and the mixture was allowed to stand for 5 h. The device was then started, and the first solenoid valve 3 and the second solenoid valve 4 were opened. The preset volume of liquid was drawn into the separatory funnel. After the liquid was drawn, the extraction was completed. The shaking rack 2 is activated to shake and extract the liquid in the separatory funnel for the preset time. Shaking stops, and after 5 hours of settling, the liquid separates into layers. Then, the third solenoid valve 10 and image acquisition unit 12 at the separatory funnel outlet are opened, and the four-way valve 11 switches to outlet c. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition unit 12 slides downwards along the slide bar 13 to monitor and identify the phase interface and liquid surface positions in the separatory funnel, acquiring images of the separatory funnel and identifying the phase interface positions. When the electromagnetic flowmeter detects that the flow rate reaches the preset 3 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 40 mL, the four-way valve switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction cycle.

[0113] The fluorine content in the sample before extraction was 83.3 mg / L, and the fluorine content in the sample after extraction was 12.4 mg / L.

[0114] Application Example 7

[0115] The α-olefin polymerization product was placed in the sample storage 5. A sodium carbonate solution with a mass fraction of 4% ethylene glycol was added to the extraction solution storage 6. The hard needles at the beginning of the first and second suction tubes were placed in the sample storage 5 and the extraction solution storage 6, respectively. The preset sample volume to be extracted was 300 mL, the extractant volume was 6 mL, the upper clear liquid (oil) volume was 40 mL, and the lower clear liquid (ethylene glycol) volume was 3 mL. The shaking frequency was 260 rpm, the shaking time was 20 min, and the mixture was allowed to stand for 10 h. The device was then started, the first solenoid valve 3 and the second solenoid valve 4 were opened, and the preset volume of liquid was drawn into the separatory funnel. After the liquid was drawn, the extraction was completed. The shaking rack 2 is activated to shake and extract the liquid in the separatory funnel for the preset time. Shaking stops, and after standing for 10 hours to allow stratification, the third solenoid valve 10 and image acquisition unit 12 at the separatory funnel outlet are opened. The four-way valve 11 is switched to outlet c, and the lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition unit 12 slides downwards along the slide bar 13 to monitor and identify the phase interface and liquid surface position in the separatory funnel, acquiring images of the separatory funnel and identifying the phase interface position. When the electromagnetic flowmeter detects that the flow rate reaches the preset 3 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit detects that the mixed liquid at the phase interface has been completely discharged from the separatory funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 40 mL, the four-way valve switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction cycle.

[0116] The fluorine content in the sample before extraction was 157.3 mg / L, and the fluorine content in the sample after extraction was 3.1 mg / L.

[0117] Comparative Example 1

[0118] The α-olefin polymerization product to be extracted is placed in the sample storage 5. An ethylene glycol solution without sodium carbonate or potassium carbonate is added to the extraction liquid storage 6. The hard needles at the beginning of the first and second suction tubes are placed in the sample storage 5 and the extraction liquid storage 6, respectively. The preset sample volume to be extracted is 20 mL, the extract volume is 8 mL, the upper clear liquid (oil) volume is 10 mL, and the lower clear liquid (alcohol) volume is 5 mL. The shaking frequency is 150 rpm, the shaking time is 10 min, and the mixture is allowed to stand for 5 h to separate. The device is then started, the first solenoid valve 3 and the second solenoid valve 4 are opened, and the preset volume of liquid is drawn into the separatory funnel. After the liquid is drawn, the extraction is completed. The shaking rack 2 is started to shake and extract the liquid in the separatory funnel for a preset time of 10 minutes. After shaking stops and the mixture is allowed to stand for 5 hours to separate into layers, the third solenoid valve 10 and the image acquisition component 12 at the outlet of the separatory funnel are opened, and the four-way valve 11 is switched to outlet C. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition component 12 slides down along the slide bar 13 to monitor and identify the phase interface and liquid surface position in the separatory funnel, and acquires the image of the separatory funnel and identifies the phase interface position. When the electromagnetic flowmeter detects that the flow rate reaches the preset 5 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit recognizes that the mixed liquid at the phase interface has been completely discharged from the separating funnel, it switches to outlet d to discharge the upper clear liquid into the upper clear liquid collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 10 mL, the four-way valve switches to outlet a, and the remaining liquid is discharged into the waste liquid collector 9, completing one extraction. If it is necessary to extract the liquid again after extraction, the first and second suction lines can be directly inserted into their respective collectors to suction the liquid.

[0119] The fluorine content in the α-olefin polymerization product before extraction was 83.3 mg / L, and the fluorine content after extraction was 79.5 mg / L.

[0120] Comparative Example 2

[0121] The α-olefin polymerization product to be extracted is placed in sample storage 5. An ethylene glycol solution without sodium carbonate or potassium carbonate is added to extraction liquid storage 6. The hard needles at the beginning of the first and second suction tubes are placed in sample storage 5 and extraction liquid storage 6, respectively. The preset volume of sample to be extracted is 10 mL, the volume of extraction liquid is 100 mL, the volume of upper clear liquid (oil) is 7 mL, and the volume of lower clear liquid (alcohol) is 30 mL. The shaking frequency is 150 rpm, the shaking time is 10 min, and the mixture is allowed to stand for 5 h to separate. The device is then started, the first solenoid valve 3 and the second solenoid valve 4 are opened, and the preset volume of liquid is drawn into the separatory funnel. After the liquid is drawn, the extraction is completed. The shaking rack 2 is started to shake and extract the liquid in the separatory funnel for a preset time of 10 minutes. After shaking stops and the mixture is allowed to stand for 5 hours to separate into layers, the third solenoid valve 10 and the image acquisition component 12 at the outlet of the separatory funnel are opened, and the four-way valve 11 is switched to outlet C. The lower layer liquid gradually flows into the lower clear liquid collector 7. At this time, the image acquisition component 12 slides down along the slide bar 13 to monitor and identify the phase interface and liquid surface position in the separatory funnel, and acquires the image of the separatory funnel and identifies the phase interface position. When the electromagnetic flowmeter detects that the flow rate reaches the preset 30 mL, the four-way valve 11 switches to outlet a to discharge the mixed liquid at the phase interface into the waste liquid collector 9. When the image acquisition unit recognizes that the mixed liquid at the phase interface has been completely discharged from the separating funnel, it switches to outlet d to discharge the supernatant into the supernatant collector 8. When the electromagnetic flowmeter detects that the flow rate reaches the preset 7 mL, the four-way valve switches to outlet a to discharge the remaining liquid into the waste liquid collector 9, completing one extraction. If it is necessary to extract the liquid again after extraction, the first and second suction lines can be directly inserted into their respective collectors to suction the liquid.

[0122] The fluorine content in the α-olefin polymerization product before extraction was 83.3 mg / L, and the fluorine content after extraction was 16.5 mg / L.

[0123] The parameters and effect data of the above application examples and comparative examples are shown in Table 1.

[0124] Table 1

[0125]

[0126] For Application Examples 1, 2, and 3, at the same extraction ratio, increasing the sodium carbonate concentration in the ethylene glycol extractant resulted in better extraction. When the sodium carbonate concentration increased to 4%, it also showed good extraction performance for samples with higher concentrations. For multiple extractions, three extractions were sufficient to complete the extraction and obtain excellent results.

[0127] Analysis of Application Examples 5 and 7, and Application Examples 1 and 6 shows that, under the same sample concentration and extraction ratio, the extraction effects of adding sodium carbonate and potassium carbonate to the ethylene glycol extractant are similar.

[0128] Comparing Application Example 1, Application Example 4, and Comparative Example 1, the extraction effect was better when the concentration of sodium carbonate in the ethylene glycol extractant was increased from 0.1% to 4%; however, the extraction effect was significantly different when pure ethylene glycol without added sodium carbonate was used for extraction; as in Comparative Example 2, the extraction effect was improved by further increasing the amount of extractant used, but it was still not as good as the effects of Application Example 1 and Application Example 4.

[0129] Obviously, the above embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the implementation of the present invention. For those skilled in the art, other variations or modifications can be made based on the above description. It is impossible to exhaustively list all the implementation methods here. All obvious variations or modifications derived from the technical solutions of the present invention are still within the protection scope of the present invention.

Claims

1. A method for the automatic extraction and separation of boron trifluoride from an alpha-olefin polymerization product, wherein, The automatic extraction separation method is completed by using an automatic extraction separation device; The automatic extraction separation device comprises an extraction unit, an image acquisition unit, a control unit, a sample reservoir (5), an extraction liquid reservoir (6), a lower clear liquid collector (7), an upper clear liquid collector (8) and a waste liquid collector (9). The sample reservoir (5) stores the α-olefin polymerization product to be extracted, and the extraction liquid reservoir (6) stores an extraction liquid prepared by mixing an alcohol and an inorganic base; the alcohol is ethylene glycol, and the inorganic base is sodium carbonate and / or potassium carbonate. The sample reservoir (5) and the extraction liquid reservoir (6) are connected with the feeding port of the extraction unit through pipelines; the discharging ports of the extraction unit are respectively connected with the lower clear liquid collector (7), the upper clear liquid collector (8) and the waste liquid collector (9); and the extraction unit is within the image acquisition range of the image acquisition unit. The control unit controls the sample reservoir (5) and the extraction liquid reservoir (6) to respectively input the α-olefin polymerization product to be extracted and the extraction liquid with preset volumes into the extraction unit, controls the extraction unit to perform oscillation mixing for a preset time length and static stratification for a preset time length, controls the image acquisition unit to acquire the image of the extraction unit and identify the position of the phase interface, and controls the extraction unit to discharge liquid based on the identified position of the phase interface. The discharging liquid comprises discharging a preset volume of lower liquid into the lower clear liquid collector (7), discharging the remaining lower liquid and mixed liquid at the phase interface into the waste liquid collector (9), and discharging a preset volume of upper liquid into the upper clear liquid collector (8). The automatic extraction separation method comprises the following processes: The preset volume of the α-olefin polymerization product to be extracted and the extraction liquid are input into the extraction unit, oscillation mixing is performed for a preset time length, static stratification is performed for a preset time length, and then the discharging liquid is performed.

2. The automated extraction separation method of claim 1, wherein, The automatic extraction separation device further comprises an input unit for inputting the preset volumes and the preset time lengths into the control unit.

3. The automated extraction separation method of claim 2, wherein, The automatic extraction separation device further comprises a display unit for displaying the input signals and state information of the control unit.

4. The automated extraction separation method of claim 1, wherein, The extraction unit comprises an extraction container (1) and an oscillation frame (2), and the extraction container (1) is installed on the oscillation frame (2).

5. The automated extraction separation method of claim 4, wherein, The sample reservoir (5) and the extraction liquid reservoir (6) are respectively connected with the top inlet of the extraction container (1) through a first liquid suction pipeline and a second liquid suction pipeline; and a pump and an electromagnetic valve are arranged on the first liquid suction pipeline and the second liquid suction pipeline.

6. The automated extraction separation method of claim 4, wherein, An electromagnetic valve is arranged at the bottom outlet of the extraction container (1), and the bottom outlet of the extraction container (1) is connected with the lower clear liquid collector (7), the upper clear liquid collector (8) and the waste liquid collector (9) through a four-way valve (11), and an electromagnetic flowmeter is arranged on the connecting pipelines.

7. The automated extraction separation method of claim 4, wherein, The image acquisition unit comprises a slide rod (13) and an image acquisition component (12) which is slidably installed on the slide rod (13); and the slide rod (13) is vertically parallel to the extraction container (1).

8. The automated extraction separation method of claim 7, wherein, The distance between the image acquisition component (12) and the extraction container (1) is 10-100 cm.

9. The automated extraction separation method of claim 1, wherein, An upper liquid outlet is arranged above the supernatant collector (8) and is connected with the feed inlet of the extraction unit.

10. The automated extraction separation method of claim 1, wherein, The mass percentage of sodium carbonate and / or potassium carbonate in the extraction liquid is 0.1%-4%.

11. The automated extraction separation method of claim 1, wherein, The volume ratio of the extraction liquid to the α-olefin polymerization product to be extracted is 1:(1-50).

12. The automated extraction separation method of claim 1, wherein, During the liquid discharge process, the preset volume of the lower layer liquid discharged into the lower layer liquid collector (7) is not greater than the input volume of the extraction liquid. The preset volume of the upper layer liquid discharged into the upper layer liquid collector (8) is not greater than the input volume of the α-olefin polymerization product to be extracted.

13. The automated extraction separation method of claim 1, wherein, When multiple extractions are required, the upper layer supernatant collected in the upper layer supernatant collector (8) is transferred to the extraction container (1) of the extraction unit for repeated extraction.

Images