Cable material cross-linking agent infiltration system and method

Abstract

The invention provides a cable material cross-linking agent infiltration system and method. The system comprises a cross-linking agent dissolving tank, at least one first flow channel, an infiltration bin and spraying equipment, the spraying equipment is arranged at the top of the infiltration bin, the cross-linking agent dissolving tank is communicated with the spraying equipment through a first flow channel, and a filter screen is arranged in the first flow channel; the spraying equipment can adjust and control the particle size of sprayed spraying particles and is used for spraying an impregnating compound into the impregnating bin; and the infiltrating bin is used for infiltrating the cable material in the infiltrating bin by using spraying particles sprayed by spraying equipment. The cable material cross-linking agent infiltration method comprises the following steps: mixing a cross-linking agent with an organic solvent to prepare an infiltration agent; the target cable material is leached and infiltrated for at least one time by using an impregnating compound; the primary leaching and infiltration treatment comprises the following steps: forming spray particles with the particle size of 10-50 microns by using an infiltration agent, spraying the spray particles onto a target cable material, forming spray particles with the particle size of 3-10 microns by using the infiltration agent, and spraying the spray particles onto the target cable material.

Description

Technical Field

[0001] This invention belongs to the field of polyethylene cable material processing technology, specifically relating to a device for determining the degree of crosslinking agent impregnation in cable materials and a method for impregnating cable materials with crosslinking agent. Background Technology

[0002] Cross-linked polyethylene (XLPE) has become one of the most commonly used insulation materials in power systems. Cross-linking is a key process for improving the performance of polyethylene, significantly enhancing its insulation properties. Increasing the degree of cross-linking in XLPE can significantly improve the insulation's breakdown resistance, as the three-dimensional network structure formed by cross-linking enhances its resistance to extrusion deformation in the direction of the electric field. The degree of cross-linking is directly related to the wetting effect of the cross-linking agent. Existing cable materials often utilize the low melting point of peroxides to impregnate polyethylene particles, adjusting the degree of cross-linking by controlling the impregnation time and temperature. Currently, XLPE cable materials generally suffer from insufficient impregnation, specifically manifested as incomplete and uneven absorption of the cross-linking agent by the material, which seriously affects the quality of power cables.

[0003] Furthermore, the traditional method for detecting the degree of peroxide infiltration mainly involves testing the gel content. This method requires first cross-linking the cross-linked polyethylene, followed by high-temperature extraction with chemical reagents to obtain the gel formed after cross-linking. Finally, the weight of the gel is weighed to calculate the gel content. This method is cumbersome and requires a long testing interval, making it impossible to provide timely feedback on the degree of infiltration.

[0004] CN105300829A discloses a method for rapidly detecting the insulation quality performance of cross-linked polyethylene (XLPE) cables, using the peak temperature of the oxygen uptake peak of XLPE in the TGA curve as a parameter for evaluating the insulation quality performance of XLPE cables. The instrument automatically saves the thermogravimetric analysis (TGA) data; based on the automatically saved TGA data and the judgment made by the instrument: for new products with a peak temperature T of not less than 240℃ for the main insulation of the cable, its main insulation thermal elongation performance is considered qualified.

[0005] CN108414459A discloses a method for detecting the crosslinking degree of crosslinked starch. This method utilizes the colorimetric reaction of starch; prepares a blank solution; performs absorbance measurement; and calculates the crosslinking degree: the crosslinking degree CL%, the average absorbance A of the original starch, and the average absorbance a of the crosslinked starch are determined by the following formula: CL% = [(Aa) / A] × 100%. Compared with traditional methods, this method is sensitive, efficient, scientific, and convenient, enabling the detection of the crosslinking degree of crosslinked starch over a wider range with greater safety.

[0006] CN102183539A discloses a method for rapidly detecting the structure of cross-linked polyethylene (XLPE) cable insulation material. Its features include detecting the crystallinity, crystal thickness, and distribution of XLPE cable material using a thermal grading method, and detecting the elastic modulus and entanglement density of XLPE cable material under high-temperature conditions using a dynamic mechanical method. Combining these two methods, a simple and effective method for detecting the structure of XLPE cable insulation material is provided.

[0007] CN110168359A discloses a method for detecting residual crosslinking aids in a crosslinked resin molded body, comprising: a heating step, wherein the crosslinked resin molded body is heated at a temperature of 500°C or higher and 700°C or lower for 3 seconds or more and 30 seconds or less; a gas analysis step, wherein the gas generated in the heating step is subjected to gas chromatography analysis; and a detection step, wherein unreacted crosslinking aids are detected based on peaks originating from residual crosslinking aids in the chromatogram obtained in the gas analysis step.

[0008] CN115343187A discloses a novel method for determining the gel content in polymers. A certain mass of sample is weighed and placed into a pre-weighed filter cartridge, which is then placed at the bottom of the extraction tube in a Soxhlet extractor. A certain volume of solvent is added to the flask, and extraction is performed under heating in a water bath. The number of extractions is recorded, and extraction is terminated when the specified number of extractions is reached. The filter cartridge is then removed and dried at a specified temperature until its mass is constant. The gel content is calculated based on the mass fraction of the gel relative to the sample mass. Compared to traditional methods that simply control the total extraction time, the gel content determined using this method is unaffected by environmental conditions, significantly shortening the determination time and improving detection efficiency while ensuring accurate results.

[0009] In short, existing detection technologies generally suffer from problems such as the inability to directly obtain the degree of oxide wetting and / or cumbersome acquisition process and poor timeliness, resulting in the inability to provide timely feedback on the degree of wetting. This is not conducive to solving the problem of incomplete and uneven absorption of cross-linking agents by materials commonly found in cross-linked polyethylene cable materials.

[0010] In summary, there is a current need to research new crosslinking agent impregnation technologies for cable materials to address the problem that the incomplete and uneven absorption of crosslinking agents by the materials in crosslinked polyethylene cable materials affects the degree of crosslinking. Summary of the Invention

[0011] The purpose of this invention is to provide a technical solution for impregnating cable materials with crosslinking agents that can alleviate the problem of incomplete or uneven absorption of crosslinking agents affecting the degree of crosslinking during the impregnation process.

[0012] To address the above problems, the present invention provides the following two technical solutions.

[0013] In a first aspect, the present invention provides a crosslinking agent impregnation system for cable materials, wherein the system includes a crosslinking agent dissolving tank, at least one first flow channel, an impregnation chamber, and a spraying device;

[0014] The spraying equipment is located at the top of the impregnation chamber, and the crosslinking agent dissolution tank is connected to the spraying equipment through the first flow channel;

[0015] The crosslinking agent dissolving tank is equipped with an organic solvent inlet, a crosslinking agent inlet, and a mixing device. The crosslinking agent dissolving tank is used to prepare the wetting agent for the crosslinking agent impregnation of cable materials. The wetting agent includes a crosslinking agent and an organic solvent. A filter screen is installed in the first flow channel. The spraying device is used to spray the wetting agent into the impregnation chamber. The spraying device can achieve adjustable particle size of the sprayed particles. The impregnation chamber is used to impregnate the cable materials placed inside using the sprayed particles from the spraying device.

[0016] The technical solution provided by this invention enables the crosslinking agent diluted with organic solvent to be sprayed with different particle sizes to sequentially impregnate cable material, thereby making the crosslinking agent distribution more uniform, making the crosslinking agent and the internal particles of the cable material more fully contacted, increasing the amount of crosslinking agent absorbed by the cable material, and improving the impregnation effect.

[0017] According to a preferred embodiment of the first aspect, the impregnation chamber is provided with a sample outlet; the cable material crosslinking agent impregnation system further includes a sample pretreatment unit and a fluorescence detection unit; the sample outlet is connected to the inlet of the sample pretreatment unit, and the outlet of the sample pretreatment unit is connected to the inlet of the fluorescence detection unit; the fluorescence detection unit can detect the degree of impregnation.

[0018] The sample pretreatment unit is equipped with a low-temperature pulverizing device and a powder washing device connected in sequence. The low-temperature pulverizing device is used to pulverize the material from the sample outlet of the immersion chamber at a temperature not exceeding -30°C. The powder washing device is used to restore the pulverized material from the low-temperature pulverizing device to room temperature, then rinse it with an organic solvent and filter and concentrate the rinsing solution.

[0019] Furthermore, the sample outlet and the sample pretreatment unit inlet are connected by a conveyor belt;

[0020] Furthermore, the fluorescence detection unit includes a fluorescence detector, a xenon lamp, a signal processing converter, and an input and display device; the fluorescence detector is provided with a housing and a sample chamber, a slit, a filter, and a light source disposed inside the housing; the housing is provided with a controllable opening and closing lid;

[0021] The signal processing converter is connected to the fluorescence detector, and the input and display device is connected to the signal processing converter, so that the data acquired by the fluorescence detector is processed by the signal processing converter and displayed on the input and display device, and the information input through the input and display device is processed by the signal processing converter and fed back to the fluorescence detector to control the fluorescence detector;

[0022] In this preferred technical solution, the degree of wetting of cable material that has undergone at least one rinsing and wetting treatment in the rinsing chamber can be tested. If the degree of wetting meets the requirements, there is no need to perform another rinsing and wetting treatment. If the degree of wetting does not meet the requirements, another rinsing and wetting treatment is performed.

[0023] According to a preferred embodiment of the first aspect, the cable material crosslinking agent impregnation system further includes an impregnation agent recovery tank, a vaporization device, and a solvent condensation and liquefaction tank.

[0024] The sizing agent recovery tank is connected to the impregnation chamber and is used to recover the sizing agent after impregnation in the impregnation chamber; the gasification equipment is connected to the sizing agent recovery tank and is used to pressurize and extract the sizing agent in the sizing agent recovery tank to vaporize the organic solvent in the sizing agent; the solvent condensation and liquefaction tank is connected to the sizing agent recovery tank and is used to allow the gaseous components in the sizing agent recovery tank to enter the solvent condensation and liquefaction tank for condensation; the solvent condensation and liquefaction tank is connected to the crosslinking agent dissolution tank and is used to allow the liquid phase product obtained from the liquefaction in the solvent condensation and liquefaction tank to enter the crosslinking agent dissolution tank for organic solvent reuse.

[0025] In this preferred embodiment, the organic solvent purification of the recovered wetting agent is effectively achieved by using a gasification device in conjunction with a solvent condensation and liquefaction tank. The recovered wetting agent is gasified using the gasification device. Due to the characteristics of organic solvents being volatile and having low boiling points, the organic solvents can be extracted from the wetting agent. The organic solvents extracted from the wetting agent are then condensed to achieve both recovery and further purification.

[0026] Furthermore, the wetting agent recovery tank is located below the impregnation chamber, and the wetting agent recovery tank and the impregnation chamber are connected by a one-way hole. The one-way hole can allow fluid to enter the wetting agent recovery tank from the impregnation chamber but not from the wetting agent recovery tank into the impregnation chamber.

[0027] Furthermore, the solvent condensation and liquefaction tank is located above the crosslinking agent dissolution tank, and the solvent condensation and liquefaction tank and the crosslinking agent dissolution tank are connected by a controllable switch filter screen;

[0028] Furthermore, the solvent condensation and liquefaction tank can achieve condensation to -20°C to -40°C and -50°C to -70°C;

[0029] Furthermore, the solvent condensation and liquefaction tank and the wetting agent recovery tank are connected by at least two gas transmission pipelines;

[0030] Furthermore, a gas regulating valve is installed on the connecting pipe between the solvent condensation and liquefaction tank and the wetting agent recovery tank.

[0031] According to a preferred embodiment of the first aspect, the mixing equipment for the crosslinking agent dissolution tank is a stirrer.

[0032] According to a preferred embodiment of the first aspect, a pressure sensor is provided in the first flow channel.

[0033] According to a preferred embodiment of the first aspect, the size of the filter screen in the first flow channel is adjustable and removable.

[0034] According to a preferred embodiment of the first aspect, the spraying device is capable of spraying spray particles with a particle size of 50 micrometers to 10 micrometers and spray particles with a particle size of 10 micrometers to 3 micrometers.

[0035] In one specific embodiment, the spraying device can spray a solution from a spray hole to form spray particles with a diameter of 50 micrometers to 10 micrometers under normal pressure using the liquid's own pressure, and can spray a solution from a spray hole to form spray particles with a diameter of 10 micrometers to 3 micrometers using pressurization.

[0036] According to a preferred embodiment of the first aspect, the pore size of the filter screen in the first flow channel is 80 micrometers to 120 micrometers.

[0037] In a second aspect, the present invention provides a method for impregnating cable material with a crosslinking agent, the method being performed using the cable material crosslinking agent impregnation system provided in the first aspect, the method comprising:

[0038] Preparation steps of the sizing agent: The crosslinking agent for cable material crosslinking agent impregnation is mixed with an organic solvent to prepare the sizing agent for cable material crosslinking agent impregnation;

[0039] Impregnation treatment steps: The target cable material shall be impregnated with an impregnating agent at least once;

[0040] The single rinsing and soaking treatment includes:

[0041] The wetting agent is used to form spray particles with a particle size of 50 micrometers to 10 micrometers, which are then sprayed onto the target cable material. Then, the wetting agent is used again to form spray particles with a particle size of 10 micrometers to 3 micrometers, which are then sprayed onto the target cable material, thereby achieving a one-time rinsing and wetting treatment of the crosslinking agent on the cable material.

[0042] According to a preferred embodiment of the second aspect, the organic solvent includes at least one selected from diethyl ether, ethanol, toluene, dichloromethane, and chloroform.

[0043] Furthermore, dichloromethane was chosen as the organic solvent.

[0044] According to a preferred embodiment of the second aspect, the crosslinking agent includes at least one of α,α-bis(tert-butylperoxy)diisopropylbenzene, tert-butyl peroxide, di-tert-butyl peroxide, triallyl cyanurate, triallyl isocyanurate, trimethylolpropane trimethacrylate, and polytriallyl isocyanurate.

[0045] Furthermore, dicumyl peroxide is selected as the crosslinking agent.

[0046] According to a preferred embodiment of the second aspect, the concentration of the crosslinking agent is 0.5%-0.8% based on 100% by weight of the wetting agent.

[0047] According to a preferred embodiment of the second aspect, the method for impregnating the cable material with a crosslinking agent further includes:

[0048] Organic solvent recycling: Collect the sprayed impregnating agent; pressurize and evacuate the collected impregnating agent to vaporize the organic solvent in the impregnating agent; condense the vaporized gaseous product to obtain organic solvent that can be recycled for impregnating agent preparation.

[0049] Furthermore, the condensation treatment of the gaseous products obtained from gasification includes:

[0050] The gaseous products obtained from gasification are condensed once at -20℃ to -40℃, and then condensed a second time at -50℃ to -70℃ to complete the condensation treatment of the gaseous products obtained from gasification.

[0051] According to a preferred embodiment of the second aspect, the impregnation step includes subjecting the target cable material to at least two rinsing impregnation treatments using an impregnating agent.

[0052] According to a preferred embodiment of the second aspect, the method for impregnating the cable material with a crosslinking agent further includes:

[0053] Testing steps: Test the degree of wetting of the target cable material after the impregnation treatment step; if the degree of wetting of the target cable material meets the standard, the impregnation of the target cable material is completed; if the degree of wetting does not meet the standard, perform another rinse and impregnation treatment, and test the degree of wetting again after the rinse and impregnation treatment, until the degree of wetting of the target cable material meets the standard, and the impregnation of the target cable material is completed.

[0054] The wetting degree detection process includes: sampling the target cable material to obtain a test sample; pulverizing the test sample using a low-temperature brittle fracture method; washing the pulverized test sample with an organic solvent; filtering and concentrating the resulting liquid phase; introducing the concentrated liquid phase into a cuvette in the sample chamber of a fluorescence detector; adding a fluorescence probe to the cuvette; turning on a light source with a wavelength compatible with the fluorescence probe; detecting the crosslinking agent content using a fluorescence detection unit; obtaining the mass of the crosslinking agent in the concentrated liquid phase by combining the detected crosslinking agent content with the volume of the concentrated liquid phase; and determining the crosslinking agent content in the test sample based on the mass of the crosslinking agent in the concentrated liquid phase and the mass of the test sample, thus completing the wetting degree determination.

[0055] During the detection of crosslinking agent content using a fluorescence detector, a light source with a wavelength compatible with the fluorescent probe is turned on. When the fluorescent probe absorbs light with the same characteristic frequency, some electrons in the atom transition from the lowest vibrational energy level in the ground state to higher vibrational energy levels. These electrons collide with similar or other molecules, consuming considerable energy, and thus descend to the lowest vibrational energy level in the first electronic excited state. From this lowest vibrational energy level, they descend to different energy levels in the ground state, emitting light with a lower frequency and longer wavelength than the previously absorbed light – this is fluorescence. The fluorescence detection unit calculates the amount of fluorescent probe consumed in the concentrated liquid phase of the cuvette sample based on the changes in fluorescence intensity. Data collection stops when all the original fluorescence disappears, and the data is converted and output to obtain the crosslinking agent content in the concentrated liquid phase. Different ratiometric fluorescent probes have specific transfer selectivity; the conversion ratio is determined by the correspondence between the selected ratiometric fluorescent probe structure and the peroxide decomposition products.

[0056] Furthermore, during the sampling process of the target cable material, point sampling is adopted; even further, the number of particles sampled each time is no less than 10; point sampling can effectively avoid the problem of incomplete test results;

[0057] Furthermore, the sample is pulverized using a low-temperature brittle fracture method by means of dry ice and ethanol at -30°C to -140°C (e.g., -72°C).

[0058] Furthermore, the organic solvent used in the washing process of the pulverized sample with an organic solvent includes at least one of diethyl ether, ethanol, toluene, dichloromethane, and chloroform; even further, the organic solvent used in the washing process of the pulverized sample with an organic solvent is dichloromethane.

[0059] Furthermore, the organic solvent used in the washing process of the pulverized sample is the same type of organic solvent as that in the wetting agent;

[0060] Furthermore, the fluorescent probe includes at least one of rhodamine-based nitrogen oxides, boron dipyrrole-based nitrogen oxides, fluorescein-based nitrogen oxides, fluorescein isothiocyanate-based nitrogen oxides, and anthocyanin fluorescent nitrogen oxides; even further, the fluorescent probe is selected from boron dipyrrole-based nitrogen oxides;

[0061] Furthermore, the liquid phase obtained after washing is filtered and then concentrated to 2 mL.

[0062] According to a preferred embodiment of the second aspect, in the single rinsing and impregnation process, a spraying device is used to spray the impregnating agent from the spray hole under normal pressure using the pressure of the impregnating agent itself to form spray particles with a particle size of 50 micrometers to 10 micrometers; or a spraying device is used to spray the impregnating agent from the spray hole under pressure to form spray particles with a particle size of 10 micrometers to 3 micrometers.

[0063] In the process of using a spraying device to atomize a wetting agent into spray particles with a diameter of 50 micrometers to 10 micrometers under normal pressure, the relationship between flow rate and pressure is crucial. The lower pressure limit is set to 20-30 MPa. When the pressure reaches the lower limit, the flow rate gradually decreases. The spray equipment is ready to use pressurization to spray the wetting agent from the spray hole to form spray particles with a diameter of 10 micrometers to 3 micrometers.

[0064] During a single rinsing and impregnation process, the sprayed particles onto the target cable material are subject to the Stokes formula for free settling of particles in still water: u = gd 2 (ρs-ρ)÷18μ; where u is the particle settling velocity (cm / s); ρs and ρ are the densities of the particles and water, respectively (g / cm); g is the gravitational acceleration (cm / s); μ is the water adhesion coefficient (Pa·s); and d is the particle diameter (cm). This formula can be used to analyze particle size and settling velocity. When the physical parameters of the substance remain constant, the particle size is directly proportional to the velocity. By utilizing the settling velocity of the particles, wetting uniformity can be better achieved, ensuring segmented wetting during a single spraying process.

[0065] Compared with the prior art, the technical solution provided by the present invention has the following beneficial effects:

[0066] 1. The technical solution provided by the present invention utilizes crosslinking agent diluted with organic solvent to sequentially impregnate cable material with spray particles of different particle sizes, thereby making the crosslinking agent distribution more uniform, making the crosslinking agent and the internal particles of the cable material more fully contacted, increasing the amount of crosslinking agent absorbed by the cable material, and improving the impregnation effect.

[0067] 2. The technical solution provided by the present invention increases the contact area between the crosslinking agent and the cable material by using solvent dilution, so that the crosslinking agent and the internal particles of the cable material can be in more sufficient contact, thereby increasing the absorption of the cable material and improving the wetting effect.

[0068] 3. The technical solution provided by the present invention utilizes crosslinking agents diluted with organic solvents to sequentially spray cable materials with spray particles of different sizes. The multiple spraying processes provide sufficient time for each stage to stand, thereby enhancing the molecular diffusion ability of the additives and further improving the effect of the additives penetrating deeper into the cable materials. At the same time, it reduces the process time and increases production capacity.

[0069] 4. In the preferred technical solution provided by the present invention, the organic solvent purification and recovery of the used wetting agent is effectively achieved by combining vaporization and condensation, thereby realizing the reuse of organic solvent, which has obvious advantages in reducing energy consumption and cost.

[0070] 5. In the preferred embodiment of the technical solution provided by the present invention, the degree of crosslinking agent impregnation of the cable material is detected online during the impregnation of the cable material, making the impregnation of the cable material more timely and accurate. Attached Figure Description

[0071] Figure 1 This is a schematic diagram of the cable material crosslinking agent impregnation system in Example 1.

[0072] Figure 2 This is a schematic diagram of the spray nozzle structure of the spray device in Example 1.

[0073] Figure 3 This is a schematic diagram of the sample pretreatment unit in Example 1.

[0074] Figure 4 This is a schematic diagram of the transmission belt structure in Example 1.

[0075] Figure 5 This is a schematic diagram of the fluorescence detector in Example 1. Detailed Implementation

[0076] In order to provide a clearer understanding of the technical features, objectives and beneficial effects of the present invention, the technical solution of the present invention will now be described in detail below, but it should not be construed as limiting the scope of implementation of the present invention.

[0077] Example 1

[0078] This embodiment provides a cable material crosslinking agent impregnation system, such as... Figure 1 As shown, the system includes:

[0079] Solvent condensation and liquefaction tank 1, crosslinking agent dissolution tank 2, six first flow channels 3, spray equipment 4, wetting chamber 5, sample pretreatment unit 6, fluorescence detection unit 7, vaporization equipment 8, wetting agent recovery tank 9, and gas transmission pipeline 10;

[0080] The crosslinking agent dissolving tank 2 is equipped with an organic solvent inlet, a crosslinking agent inlet, and a mixing device. The mixing device is a stirrer. The crosslinking agent dissolving tank 2 is used to prepare the impregnating agent for the crosslinking agent impregnation of cable materials. The impregnating agent includes a crosslinking agent and an organic solvent. The first flow channel 3 is equipped with a pressure sensor and an adjustable and removable filter screen. The pore size of the filter screen in the first flow channel is 80 micrometers to 120 micrometers.

[0081] Spraying device 4 uses a pressure-sensing spray plate, which is equipped with spray holes 12, such as... Figure 2 As shown, the spraying device 4 is located at the top of the impregnation chamber 5. The crosslinking agent dissolution pool 2 is connected to the spraying device 4 through the first flow channel 3. The spraying device 4 is used to spray the impregnation agent into the impregnation chamber 5. The spraying device 4 can achieve adjustable particle size of the sprayed particles. Specifically, it can use the liquid's own pressure to spray the solution from the spray hole 12 to form spray particles with a particle size of 50 micrometers to 10 micrometers under normal pressure, and use pressurization to spray the solution from the spray hole 12 to form spray particles with a particle size of 10 micrometers to 3 micrometers.

[0082] The impregnation chamber 5 is used to impregnate the cable material placed inside it with spray particles sprayed from the spraying device 4.

[0083] An impregnating agent recovery tank 9 is located below the impregnation chamber 5. The impregnating agent recovery tank 9 and the impregnation chamber 5 are connected via a one-way hole. This one-way hole allows fluid to enter the impregnating agent recovery tank 9 from the impregnation chamber 5 but prevents fluid from entering the impregnating chamber 5 from the impregnating agent recovery tank 9. The impregnating agent recovery tank is used to recover the impregnating agent after impregnation in the impregnation chamber 5. A vaporization device 8 is connected to the impregnating agent recovery tank 9 and is used to pressurize and extract air from the impregnating agent in the tank 9, causing the organic solvent in the impregnating agent to vaporize. A solvent condensation and liquefaction tank 1 is connected to the impregnating agent recovery tank 9 via a gas transmission pipe 10, used to achieve… The gaseous components in the wetting agent recovery tank 9 enter the solvent condensation and liquefaction tank 1 for condensation, and the gas pipeline 10 is equipped with a gas regulating valve; the solvent condensation and liquefaction tank 1 is located above the crosslinking agent dissolution tank 2, and the solvent condensation and liquefaction tank 1 and the crosslinking agent dissolution tank 2 are connected by a controllable switch filter with a pore size of 30-50 micrometers, which is used to enable the liquid phase product obtained by liquefaction in the solvent condensation and liquefaction tank 1 to enter the crosslinking agent dissolution tank 2 for organic solvent recycling; the solvent condensation and liquefaction tank 1 can achieve condensation to -20℃ to -40℃ and -50℃ to -70℃;

[0084] The immersion chamber 5 is equipped with a sample outlet 13; such as Figure 3As shown, the sample pretreatment unit 6 is equipped with a cryogenic pulverizer 19 and a powder washing device 20 connected in sequence; the sample outlet 13 and the inlet of the cryogenic pulverizer 19 in the sample pretreatment unit 6 are connected by a conveyor belt 18 (e.g., Figure 4 (As shown) Connection; The cryogenic pulverizing equipment 11 is used to pulverize the material from the sample outlet 13 of the wetting chamber 5 at a temperature not exceeding -30°C. The powder washing equipment 20 is used to restore the pulverized material from the cryogenic pulverizing equipment 19 to room temperature, then rinse it with an organic solvent and filter and concentrate the resulting solution. The outlet of the sample pretreatment unit 6 is connected to the inlet of the fluorescence detection unit 7; the fluorescence detection unit 7 can detect the degree of wetting. The fluorescence detection unit 7 includes a fluorescence detector 14, a xenon lamp 15, a signal processing converter 16, and an input and display device 17; as shown Figure 5 As shown, the fluorescence detector 14 includes a housing 21 and a sample chamber 22, a slit 23, a filter 24, and a light source 25 disposed inside the housing; the housing 21 is equipped with a controllable opening and closing cover 26. A signal processing converter 16 is connected to the fluorescence detector 14, and an input and display device 17 is connected to the signal processing converter 16, thereby enabling the fluorescence detector 14 to control the data acquired by the fluorescence detector 14, which is then processed by the signal processing converter 16 and displayed on the input and display device 17. Additionally, information input through the input and display device 17 is processed by the signal processing converter 16 and fed back to the fluorescence detector 14.

[0085] Example 2

[0086] This embodiment provides a method for impregnating cable material with a crosslinking agent, using the cable material crosslinking agent impregnation system provided in Embodiment 1. The method includes:

[0087] Preparation steps of the sizing agent: The crosslinking agent for cable material crosslinking is mixed with an organic solvent in the crosslinking agent dissolution tank 2 to prepare the crosslinking agent for cable material crosslinking; wherein, the organic solvent is dichloromethane, the crosslinking agent is dicumyl peroxide, and the crosslinking agent concentration is 0.5%-0.8% based on the mass of the sizing agent as 100%.

[0088] Impregnation treatment steps: The target cable material is impregnated twice with an impregnating agent in impregnation chamber 5;

[0089] The single rinsing and soaking treatment includes:

[0090] The wetting agent prepared in the crosslinking agent dissolution tank 2 enters the spraying device 4 through the first flow channel 3. During the process of passing through the first flow channel 3, the wetting agent is filtered by a filter screen. The spraying device 4 uses the pressure of the wetting agent itself to spray the wetting agent from the spray hole 12 under normal pressure to form spray particles with a particle size of 50 micrometers to 10 micrometers and spray them onto the target cable material. Then, the spraying device 4 uses pressure to spray the wetting agent from the spray hole 12 to form spray particles with a particle size of 10 micrometers to 3 micrometers and spray them onto the target cable material, thereby realizing the one-time rinsing and wetting treatment of the cable material crosslinking agent.

[0091] Organic solvent recycling steps: The wetting agent sprayed in the wetting chamber 5 enters the wetting agent recovery tank 9. The wetting agent in the wetting agent recovery tank 9 is pressurized and evacuated to vaporize the organic solvent in the wetting agent. The gaseous product obtained by vaporization enters the solvent condensation and liquefaction tank 1 through the gas transmission pipeline 10. The solvent condensation and liquefaction tank 1 is condensed to obtain organic solvent that can be recycled for the preparation of the wetting agent.

[0092] The condensation process in solvent condensation and liquefaction tank 1 includes:

[0093] The gaseous products obtained from gasification are condensed once at -20℃ to -40℃, and then condensed a second time at -50℃ to -70℃ to complete the condensation treatment of the gaseous products obtained from gasification.

[0094] Testing steps: Test the degree of wetting of the target cable material after the impregnation treatment step; if the degree of wetting of the target cable material meets the standard, the impregnation of the target cable material is completed; if the degree of wetting does not meet the standard, perform another rinse and impregnation treatment, and test the degree of wetting again after the rinse and impregnation treatment, until the degree of wetting of the target cable material meets the standard, and the impregnation of the target cable material is completed.

[0095] The wetting degree detection process includes: sampling the target cable material using a point sampling method, with each sampling consisting of no fewer than 10 particles, to obtain a test sample; pulverizing the test sample using a low-temperature pulverizing device 19 via a low-temperature brittle fracture method (specifically, pulverizing with dry ice and ethanol at -72°C); pulverizing the test sample and then washing it in a powder washing device 20 after it has been restored to room temperature, followed by washing with the organic solvent dichloromethane; filtering the resulting liquid phase and concentrating it to 2 mL; introducing the concentrated liquid phase into a cuvette in the sample chamber 22 of a fluorescence detector; adding a fluorescent probe, boron dipyrrole nitrogen oxide, to the cuvette; turning on a light source 25 with a wavelength compatible with the fluorescent probe; and using a fluorescence detection unit 7 to detect the crosslinking agent content; using the detected crosslinking agent content in the concentrated liquid phase combined with the volume of the concentrated liquid phase to obtain the mass of the crosslinking agent in the concentrated liquid phase; and based on the mass of the crosslinking agent in the concentrated liquid phase and the mass of the test sample, determining the crosslinking agent content in the test sample, thus completing the wetting degree determination.

[0096] Comparative Example 1

[0097] This embodiment provides a method for impregnating cable material with a crosslinking agent, using the cable material crosslinking agent impregnation system provided in Embodiment 1. The method includes:

[0098] Preparation steps of the sizing agent: The crosslinking agent for cable material crosslinking is mixed with an organic solvent in the crosslinking agent dissolution tank 2 to prepare the crosslinking agent for cable material crosslinking; wherein, the organic solvent is dichloromethane, the crosslinking agent is dicumyl peroxide, and the crosslinking agent concentration is 0.5%-0.8% based on the mass of the sizing agent as 100%.

[0099] Impregnation treatment steps: The target cable material is impregnated twice with an impregnating agent in impregnation chamber 5;

[0100] The single rinsing and soaking treatment includes:

[0101] The wetting agent prepared in the crosslinking agent dissolution tank 2 enters the spraying device 4 through the first flow channel 3. During the process of passing through the first flow channel 3, the wetting agent is filtered by a filter screen. The spraying device 4 is used to spray the wetting agent from the spray hole 12 under normal pressure using the pressure of the wetting agent itself to form spray particles with a particle size of 50 micrometers to 10 micrometers onto the target cable material, thereby realizing the one-time washing and wetting treatment of the cable material crosslinking agent.

[0102] Organic solvent recycling steps: The wetting agent sprayed in the wetting chamber 5 enters the wetting agent recovery tank 9. The wetting agent in the wetting agent recovery tank 9 is pressurized and evacuated to vaporize the organic solvent in the wetting agent. The gaseous product obtained by vaporization enters the solvent condensation and liquefaction tank 1 through the gas transmission pipeline 10. The solvent condensation and liquefaction tank 1 is condensed to obtain organic solvent that can be recycled for the preparation of the wetting agent.

[0103] The condensation process in solvent condensation and liquefaction tank 1 includes:

[0104] The gaseous products obtained from gasification are condensed once at -20℃ to -40℃, and then condensed a second time at -50℃ to -70℃ to complete the condensation treatment of the gaseous products obtained from gasification.

[0105] Testing steps: Test the degree of wetting of the target cable material after the impregnation treatment step; if the degree of wetting of the target cable material meets the standard, the impregnation of the target cable material is completed; if the degree of wetting does not meet the standard, perform another atmospheric pressure rinsing and impregnation treatment, and test the degree of wetting again after the rinsing and impregnation treatment, until the degree of wetting of the target cable material meets the standard, and the impregnation of the target cable material is completed.

[0106] The wetting degree detection process includes: sampling the target cable material using a point sampling method, with each sampling consisting of no fewer than 10 particles, to obtain a test sample; pulverizing the test sample using a low-temperature pulverizing device 19 via a low-temperature brittle fracture method (specifically, pulverizing with dry ice and ethanol at -72°C); pulverizing the test sample and then washing it in a powder washing device 20 after it has been restored to room temperature, followed by washing with the organic solvent dichloromethane; filtering the resulting liquid phase and concentrating it to 2 mL; introducing the concentrated liquid phase into a cuvette in the sample chamber 22 of a fluorescence detector; adding a fluorescent probe, boron dipyrrole nitrogen oxide, to the cuvette; turning on a light source 25 with a wavelength compatible with the fluorescent probe; and using a fluorescence detection unit 7 to detect the crosslinking agent content; using the detected crosslinking agent content in the concentrated liquid phase combined with the volume of the concentrated liquid phase to obtain the mass of the crosslinking agent in the concentrated liquid phase; and based on the mass of the crosslinking agent in the concentrated liquid phase and the mass of the test sample, determining the crosslinking agent content in the test sample, thus completing the wetting degree determination.

[0107] Experimental Example 1

[0108] The gel content of the cable material that underwent one rinse and impregnation treatment, two rinse and impregnation treatments, and three rinse and impregnation treatments in Example 2 and Comparative Example 1 was tested.

[0109] The gel content test is a commonly used method for detecting the degree of resin crosslinking. The specific method is as follows: Weigh approximately 0.3g of the sample to be tested, denoted as m1. Wrap the sample in a 0.074mm copper mesh and immerse it in xylene solution. Extract the sample at 180℃ using a reflux extractor for 4 hours. Remove the sample and wash it three times with anhydrous ethanol. Then, dry it in a vacuum drying oven at 100℃ for 2 hours. Weigh the dried sample and record the mass as m2. Use the formula... Determine the gel content (Cgel) of the sample to be tested.

[0110] The results are shown in Table 1.

[0111] Table 1

[0112]

[0113] As shown in Table 1, the crosslinking agent impregnation method for cable materials provided by the present invention, which sequentially impregnates the cable material with spray particles of different particle sizes, has a significantly better impregnation effect than sequentially impregnating the cable material with spray particles of uniform particle size.

[0114] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A crosslinking agent impregnation system for cable materials, wherein, The system includes a crosslinking agent dissolution tank, at least one first flow channel, an impregnation chamber, and a spraying device; The spraying equipment is located at the top of the impregnation chamber, and the crosslinking agent dissolution tank is connected to the spraying equipment through the first flow channel; The crosslinking agent dissolving tank is equipped with an organic solvent inlet, a crosslinking agent inlet, and a mixing device. The crosslinking agent dissolving tank is used to prepare the wetting agent for the crosslinking agent impregnation of cable materials. The wetting agent includes a crosslinking agent and an organic solvent. A filter screen is installed in the first flow channel. The spraying device is used to spray the wetting agent into the impregnation chamber. The spraying device can achieve adjustable particle size of the sprayed particles. The impregnation chamber is used to impregnate the cable materials placed inside using the sprayed particles from the spraying device.

2. The system according to claim 1, wherein, The impregnation chamber is equipped with a sample outlet; the cable material crosslinking agent impregnation system also includes a sample pretreatment unit and a fluorescence detection unit; the sample outlet is connected to the inlet of the sample pretreatment unit, and the outlet of the sample pretreatment unit is connected to the inlet of the fluorescence detection unit; the fluorescence detection unit can detect the degree of impregnation. The sample pretreatment unit is equipped with a low-temperature pulverizing device and a powder washing device connected in sequence. The low-temperature pulverizing device is used to pulverize the material from the sample outlet of the immersion chamber at a temperature not exceeding -30°C. The powder washing device is used to restore the pulverized material from the low-temperature pulverizing device to room temperature, then rinse it with an organic solvent and filter and concentrate the resulting solution.

3. The system according to claim 1, wherein, The cable material crosslinking agent impregnation system also includes an impregnation agent recovery tank, a vaporization device, and a solvent condensation and liquefaction tank; The wetting agent recovery tank is connected to the wetting chamber and is used to recover the wetting agent after wetting in the wetting chamber; the gasification equipment is connected to the wetting agent recovery tank and is used to pressurize and extract the wetting agent in the wetting agent recovery tank to vaporize the organic solvent in the wetting agent; the solvent condensation and liquefaction tank is connected to the wetting agent recovery tank and is used to allow the gas phase components in the wetting agent recovery tank to enter the solvent condensation and liquefaction tank for condensation; the solvent condensation and liquefaction tank is connected to the crosslinking agent dissolution tank and is used to allow the liquid phase products obtained from the liquefaction in the solvent condensation and liquefaction tank to enter the crosslinking agent dissolution tank for organic solvent reuse.

4. The system according to claim 3, wherein, The wetting agent recovery tank is located below the impregnation chamber. The wetting agent recovery tank and the impregnation chamber are connected by a one-way hole. The one-way hole allows fluid to enter the wetting agent recovery tank from the impregnation chamber but not from the wetting agent recovery tank into the impregnation chamber. The solvent condensation and liquefaction tank is located above the crosslinking agent dissolution tank, and the solvent condensation and liquefaction tank and the crosslinking agent dissolution tank are connected by a controllable switch filter screen.

5. The system according to claim 3, wherein, The solvent condensation and liquefaction tank can achieve condensation to -20℃ to -40℃ and -50℃ to -70℃.

6. The system according to claim 1, wherein, The spraying equipment can spray particles with a diameter of 50 micrometers to 10 micrometers and particles with a diameter of 10 micrometers to 3 micrometers. The filter screen in the first flow channel has a pore size of 80-120 micrometers.

7. A method for impregnating cable material with a crosslinking agent, the method being carried out using the cable material crosslinking agent impregnation system of any one of claims 1-6, the method comprising: Preparation steps of the sizing agent: The crosslinking agent for cable material crosslinking agent impregnation is mixed with an organic solvent to prepare the sizing agent for cable material crosslinking agent impregnation; Impregnation treatment steps: The target cable material shall be impregnated with an impregnating agent at least once; The single rinsing and soaking treatment includes: The wetting agent is used to form spray particles with a particle size of 50 micrometers to 10 micrometers, which are then sprayed onto the target cable material. Then, the wetting agent is used again to form spray particles with a particle size of 10 micrometers to 3 micrometers, which are then sprayed onto the target cable material, thereby achieving a one-time rinsing and wetting treatment of the crosslinking agent on the cable material.

8. The method according to claim 7, wherein, Organic solvents include at least one of diethyl ether, ethanol, toluene, dichloromethane, and chloroform; The crosslinking agent includes at least one of α,α-bis(tert-butylperoxy)diisopropylbenzene, tert-butyl peroxide, di-tert-butyl peroxide, triallyl cyanurate, triallyl isocyanurate, trimethylolpropane trimethacrylate, and polytriallyl isocyanurate. Based on 100% by weight of the wetting agent, the crosslinking agent concentration is 0.5%-0.8%.

9. The method according to claim 7, wherein, The crosslinking agent impregnation method for cable materials also includes: Organic solvent recycling: Collect the sprayed impregnating agent; pressurize and evacuate the collected impregnating agent to vaporize the organic solvent in the impregnating agent; condense the vaporized gaseous product to obtain organic solvent that can be recycled for impregnating agent preparation.

10. The method according to claim 9, wherein, The condensation treatment of the gaseous products obtained by gasification includes: condensing the gaseous products obtained by gasification once at -20℃ to -40℃, and then condensing them a second time at -50℃ to -70℃, thereby completing the condensation treatment of the gaseous products obtained by gasification.

11. The method according to claim 7 or 9, wherein, The crosslinking agent impregnation method for cable materials also includes: Testing steps: Test the degree of wetting of the target cable material after the impregnation treatment step; if the degree of wetting of the target cable material meets the standard, the impregnation of the target cable material is completed; if the degree of wetting does not meet the standard, perform another rinse and impregnation treatment, and test the degree of wetting again after the rinse and impregnation treatment, until the degree of wetting of the target cable material meets the standard, and the impregnation of the target cable material is completed. The wetting degree detection process includes: sampling the target cable material to obtain a test sample; pulverizing the test sample using a low-temperature brittle fracture method; washing the pulverized test sample with an organic solvent; filtering and concentrating the resulting liquid phase; introducing the concentrated liquid phase into a cuvette in the sample chamber of a fluorescence detector; adding a fluorescence probe to the cuvette; turning on a light source with a wavelength compatible with the fluorescence probe; detecting the crosslinking agent content using a fluorescence detection unit; obtaining the mass of the crosslinking agent in the concentrated liquid phase by combining the detected crosslinking agent content with the volume of the concentrated liquid phase; and determining the crosslinking agent content in the test sample based on the mass of the crosslinking agent in the concentrated liquid phase and the mass of the test sample, thus completing the wetting degree determination.

12. The method according to claim 11, wherein, The organic solvents used in the washing of the pulverized sample with organic solvents include at least one of diethyl ether, ethanol, toluene, dichloromethane, and chloroform.

13. The method according to claim 11, wherein, The organic solvent used in the washing process of the pulverized sample is the same type of organic solvent as that in the wetting agent.

14. The method according to claim 11, wherein, Fluorescent probes include at least one of rhodamine-based nitrogen oxides, boron dipyrrole-based nitrogen oxides, fluorescein-based nitrogen oxides, fluorescein isothiocyanate nitrogen oxides, and anthocyanin fluorescent nitrogen oxides.

15. The method according to claim 11, wherein, In a single rinsing and impregnation process, a spraying device is used to spray the impregnating agent from the spray hole under normal pressure, forming spray particles with a particle size of 50 micrometers to 10 micrometers; or the spraying device is used to spray the impregnating agent from the spray hole under pressure, forming spray particles with a particle size of 10 micrometers to 3 micrometers.

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