Efficient desizing device and method for ultralow-dielectric-loss electronic-grade quartz glass fiber cloth

Abstract

The invention discloses an efficient desizing device and method for ultralow-dielectric-loss electronic-grade quartz glass fiber cloth, and relates to the technical field of desizing of quartz glass fiber cloth. The mode of combining CO2 and desizing liquid is adopted, organic matter on the surface of the quartz glass fiber cloth is pre-degraded, then ultrasonic washing, spunlace, spraying and other modes are sequentially carried out to wash the organic matter, splitting is achieved, desizing time can be shortened, desizing temperature can be reduced, energy consumption is reduced, and the desizing effect is improved. And for a quartz glass fiber cloth product, the cloth cover strength loss can be reduced. Compared with the prior art that smoldering can harden the fibers and is not beneficial to splitting in the subsequent FN process, the method has the advantages that the fibers are split in the desizing process, so that the problem is solved.

Description

TECHNICAL FIELD

[0001] The application relates to the desizing technology of quartz glass fiber cloth, in particular to an efficient desizing device and method for ultra-low dielectric loss electronic-grade quartz glass fiber cloth. BACKGROUND

[0002] Quartz fiber has extremely low dielectric constant and dielectric loss, is the "ceiling" in glass fiber materials, and can improve signal transmission speed, increase signal transmission quality and reduce signal loss when applied to printed circuit boards. With the rapid development of electronic information equipment such as AI servers, star chains and automatic driving chips, the market demand for electronic-grade quartz glass fiber is showing an explosive growth trend.

[0003] Due to the hard and brittle characteristics of quartz glass fiber, starch type sizing agent and sizing agent need to be coated on the surface of the yarn to improve its wear resistance. Since the organic matter coated on the glass fiber will hinder the adhesion between the fiber and the reinforced substrate, thereby affecting the electrical properties of the downstream customer product PCB board. Therefore, generally, the sizing agent on the surface of the glass fiber is removed through a heat cleaning and post-treatment process, and then the coupling agent coating and fiber opening treatment are performed through the FN process before use. At present, the main desizing method for electronic-grade quartz glass fiber cloth is KH continuous heat treatment desizing and BH secondary desizing. For special electronic-grade quartz glass fiber cloth, this desizing method has the disadvantages of large cloth strength loss, incomplete desizing, poor cloth opening effect and the like. Chinese invention patent CN113957701B discloses a water-soluble one-step desizing solution for ultra-thin electronic-grade glass fiber cloth and a preparation method. The desizing solution comprises 6-8 parts of stabilizer, 15-20 parts of alkali, 1-3 parts of hydrogen peroxide, 2-5 parts of additive and water. The desizing solution of the patent can reduce the cloth strength loss and desize cleanly, but the high content of strong alkali in the desizing solution leads to poor cloth hair condition, which needs to be further improved. Therefore, there is an urgent need to develop an efficient desizing method for electronic-grade quartz glass fiber cloth to solve the problems existing in the above-mentioned desizing methods. SUMMARY

[0004] The technical problem to be solved by the application is to overcome the deficiencies of the prior art and provide an efficient desizing device and method for ultra-low dielectric loss electronic-grade quartz glass fiber cloth. The CO2 and desizing solution are combined to pre-desize the organic matter on the surface of the quartz glass fiber cloth, and then the organic matter is washed, spun, sprayed and opened in sequence, which can reduce the desizing time and temperature, thereby reducing the energy consumption and improving the desizing effect.

[0005] The technical scheme of the application is as follows:

[0006] In one aspect, the application provides an efficient desizing device for ultra-low dielectric loss electronic-grade quartz glass fiber cloth, comprising a CO2 desizing reactor, an ultrasonic water washing tank, a water jet mechanism, a spraying mechanism, a drying mechanism and a winding shaft, a conveying roller is arranged between the ultrasonic water washing tank, the water jet mechanism, the spraying mechanism, the drying mechanism and the winding shaft, and the quartz glass fiber cloth is conveyed through the conveying roller; the CO2 desizing reactor comprises a shell, air inlets and outlets are arranged at two ends of the shell respectively, a desizing liquid nozzle is mounted at the top of the shell, a winding shaft is arranged in the shell, and the quartz glass fiber cloth is wound on the winding shaft; the ultrasonic water washing tank comprises a water tank, a roller is arranged in the water tank, the roller is driven to rotate by a motor, water outlets are arranged on the roller, the quartz glass fiber cloth is attached to the surface of the roller, the quartz glass fiber cloth is conveyed by rolling with the roller, and an ultrasonic rod is arranged at the center of the roller; the water jet mechanism comprises a water jet pipe one, a plurality of rows of water jet holes one are arranged at the bottom of the water jet pipe one, water is sprayed on the quartz glass fiber cloth below to wash and fibrillate the residual organic matter of the quartz glass fiber cloth; and the spraying mechanism comprises a water jet pipe two, water jet holes two are arranged at the bottom of the water jet pipe two, water is sprayed on the quartz glass fiber cloth below to wash and fibrillate the residual organic matter of the quartz glass fiber cloth.

[0007] Preferably, a filter membrane is arranged at the air inlet of the CO2 desizing reactor, and a flow guide horn is arranged at the air inlet in the shell.

[0008] Preferably, a plurality of wave wheels are arranged in the roller along the length direction of the roller, and the wave wheels are driven to rotate by a motor; the water outlets on the roller have a diameter of 2-5 mm and a spacing of 5-10 mm, too large or too sparse water outlets will result in insufficient water pressure, too small or too dense water outlets will cause the quartz glass fiber cloth to be sprayed out of wrinkles, and the roller will not have enough support; two tension rollers are arranged above and below the feeding end and the discharging end of the ultrasonic water washing tank respectively, and the quartz glass fiber cloth passes between the two tension rollers; a pressing roller is arranged at the feeding end and the discharging end of the ultrasonic water washing tank respectively, so that the quartz glass fiber cloth is attached to the surface of the roller.

[0009] Preferably, the drying mechanism comprises a drying furnace, a plurality of conveying rollers are arranged in the drying furnace, and the quartz glass fiber cloth is conveyed and dried in the drying furnace through the conveying rollers.

[0010] Preferably, six rows of water jet holes one are arranged at the bottom of the water jet pipe one, the water jet holes one have a diameter of 0.05-0.1 mm and a spacing of 0.1-0.2 mm, and the distance between the water jet holes one and the quartz glass fiber cloth is 7-9 cm; one row of water jet holes two is arranged at the bottom of the water jet pipe two, the water jet holes two have a diameter of 0.4-0.5 mm and a spacing of 5-8 cm, and the distance between the water jet holes two and the quartz glass fiber cloth is 9-11 cm. If the distance between the water jet holes one and the quartz glass fiber cloth is too close, the water jet effect on the ultra-thin cloth will be too strong, which will damage the cloth surface; if the distance is too far, the water jet effect will be too weak, which will not achieve the cleaning and fibrillation effect.

[0011] In another aspect, the present application provides a high-efficiency desizing method for ultra-low dielectric loss electronic-grade quartz glass fiber cloth, which is carried out by the high-efficiency desizing device for ultra-low dielectric loss electronic-grade quartz glass fiber cloth and includes the following steps:

[0012] S1 Pre-desizing: The quartz glass fiber cloth wound on the spool is placed in the CO2 desizing reactor, the desizing solution is sprayed onto the quartz glass fiber cloth through the desizing solution nozzle, and CO2 is introduced into the CO2 desizing reactor through the gas inlet and flows out through the gas outlet; during this process, the sizing on the surface of the quartz glass fiber cloth reacts with the desizing solution and is carried away by the CO2 flow, realizing the pre-desizing of the sizing on the surface of the quartz glass fiber cloth. During this process, the desizing solution sprays cover the entire CO2 desizing reactor, effectively contacts with CO2 and forms a microemulsion, promoting the reaction of the desizing solution with the sizing and the organic matter of the sizing agent on the surface of the quartz glass fiber cloth, and accelerating the desizing of the quartz glass fiber cloth. According to the principle of similarity, the sizing on the surface of the quartz glass fiber cloth dissolves in CO2 and flows away from the surface of the quartz glass fiber cloth, and the sizing inside the quartz glass fiber cloth diffuses to the surface under the action of concentration difference, the newly introduced CO2 molecules quickly approach the surface of the quartz glass fiber cloth, so that the sizing diffused to the surface continues to dissolve in CO2 and is carried away, thereby completing the pre-desizing of the sizing.

[0013] S2 Ultrasonic water washing: the spool with the pre-desized quartz glass fiber cloth is taken out of the CO2 desizing reactor, the quartz glass fiber cloth is conveyed to the ultrasonic water washing tank through the conveying roller under the action of the winding spool, and is attached to the surface of the roller, the quartz glass fiber cloth is conveyed by rolling with the roller, at the same time, the ultrasonic waves emitted by the ultrasonic rod further clean the sizing on the surface of the quartz glass fiber cloth and the quartz glass fiber, improving the desizing effect. The ultrasonic waves emitted by the ultrasonic rod have washing, dispersing and cavitation effects, which separate the organic macromolecules on the quartz glass fiber cloth, promote the adhesion of the sizing and the sizing agent to the fiber to become loose, and reduce the surface tension of the stain, emulsify the dirt and oil; the emulsification caused by the ultrasonic waves changes the removed sizing from a gel state to a sol state, improving the desizing effect of the organic matter; the thermal effect of the ultrasonic waves keeps the water solution at a certain temperature, providing energy for the reaction, ultimately not only cleaning the surface organic matter of the quartz glass fiber cloth, but also removing the sizing mixed in the quartz glass fiber, improving the desizing effect.

[0014] S3 Hydroentanglement: the quartz glass fiber cloth after ultrasonic water washing is conveyed to the hydroentanglement mechanism through the conveying roller, water is sprayed onto the quartz glass fiber cloth through the water spraying pipe one, and the residual organic matter of the quartz glass fiber cloth is washed and fibrillated.

[0015] S4 Spraying: the quartz glass fiber cloth after hydroentanglement is conveyed to the spraying mechanism through the conveying roller, water is sprayed onto the quartz glass fiber cloth through the water spraying pipe two, and the residual organic matter of the quartz glass fiber cloth is further washed and fibrillated.

[0016] S5 drying: the sprayed quartz glass fiber cloth is conveyed to a drying mechanism by a conveying roller for drying.

[0017] S6 winding: the dried quartz glass fiber cloth is wound on a winding shaft.

[0018] Preferably, in step S1, 1000L of the desizing solution comprises the following components by mass percentage: sodium percarbonate 6.25-10.5%, tetraacetylethylenediamine 2.5-3.5%, PVA-degrading enzyme 0.35-0.5%, PEG-degrading enzyme 0.35-0.5%, amylase 0.35-0.75%, pH buffer 3.61-4.41%, penetrating agent 0.5-1.5%, anti-staining agent 14.25-21%, and the balance is pure water; wherein the pH buffer is disodium hydrogen phosphate 2.66-3.36% and citric acid 0.95-1.05%, and the anti-staining agent is 5.7-6% FMEE and 8.55-15% FMES.

[0019] In the desizing solution used in the application, sodium percarbonate can slowly decompose into sodium carbonate and hydrogen peroxide (hydrogen dioxide) in aqueous solution, and sodium carbonate can be used as an enzyme activator and provide a weak alkaline pH. Under alkaline conditions, tetraacetylethylenediamine can not only generate peracetic acid with actual bleaching effect with hydrogen peroxide, but also accelerate the decomposition of sodium percarbonate. Each 1000L of the desizing solution contains 6.25-10.5% of sodium percarbonate, and the addition amount is too small, the generated ·OH is small, the pH value is also low, and the desizing rate is reduced; and the addition amount is too large, which is beneficial to the oxidation of acetic anhydride, so as to reduce the pH value of the desizing solution and reduce the oxidation desizing efficiency.

[0020] The generated peracetic acid reduces the pH of the desizing solution, but the pH reduction is not conducive to the further activation, decomposition of hydrogen peroxide, and activity of biological enzymes. The sodium carbonate decomposed from sodium percarbonate can appropriately increase the pH of the desizing solution, so that it presents weak alkalinity at the beginning.

[0021] Both hydrogen peroxide and peracetic acid are oxidizing agents, and can oxidize the polyester fabric under alkaline conditions. ·OH decomposed from hydrogen peroxide has extremely strong oxidizing ability. For carbohydrates, under the action of ·OH, the starch molecules undergo a de-H reaction, the C-C bond is broken, and finally completely oxidized to CO2. ·OH is added to the carbon-carbon double bond of water-soluble polymer, the double bond is broken, and completely oxidized to CO2.

[0022] Preferably, the mass ratio of sodium percarbonate to tetraacetylethylenediamine is (2.5-3):1. If the ratio is too small, the generated hydrogen peroxide is insufficient, and the desizing rate decreases rapidly. If the ratio is too large, the catalyst is insufficient, and the desizing rate also decreases rapidly. In the pH buffer, the mass ratio of disodium hydrogen phosphate to citric acid is (2.8-3.2):1. If the pH is too low, the hydrogen peroxide is stable, and the decomposition of hydrogen peroxide is insufficient. If the pH is too high, the decomposition of hydrogen peroxide is too fast, which causes ineffective decomposition. When the mass ratio of disodium hydrogen phosphate to citric acid meets the above ratio, the enzyme activity is the highest at this pH. The citric acid can be used as a chelating agent to chelate metal ions in the sizing material and prevent the fabric from yellowing. The main components of the sizing material coated on the surface of the quartz glass fiber cloth are starch, polyvinyl alcohol (PVA), and polyethylene glycol (PEG). The mass ratio of PVA-degrading enzyme, PEG-degrading enzyme, and amylase is 1:1:(1-1.5). The amylase is bacterial alpha-amylase, such as Bacillus subtilis, Bacillus amyloliquefaciens, and Bacillus licheniformis. The starch is hydrolyzed into dextrin and oligosaccharide, which is easy to remove during washing. Smaller molecules often surround larger molecules, that is, PVA and PEG wrap starch. The amylase can enter the gap between PVA and PEG to act on starch. When the starch is hydrolyzed, the outer PVA and PEG are deformed and fall off the fabric. The PVA-degrading enzyme is a hydrolytic enzyme, such as Alcaligenes faecalis and Stenotrophomonas maltophilia, which degrades PVA. The PEG-degrading enzyme is an oxidation-reduction enzyme, such as Achromobacter and Bacillus, which degrades PEG. In the anti-staining agent, the mass ratio of FMEE to FMES is 1:(1.5-2.5). FMEE is an environmentally friendly non-ionic surfactant, such as octadecanoic acid fatty acid polyoxybutylene-7 ester and hexadecanoic acid fatty acid polyoxybutylene-7 ester. FMEE has strong penetration and can penetrate into the interior of the glass fiber of the fabric to accelerate the falling off of the sizing material and has strong cleaning power. FMES is a sulfonate of FMEE, such as octadecanoic acid fatty acid polyoxybutylene-7 ester sodium sulfonate and hexadecanoic acid fatty acid polyoxybutylene-7 ester sodium sulfonate. FMES is an anionic surfactant and has strong dispersion. When FMEE is used alone, the sizing material in the solution will re-stain the surface of the glass fiber as the amount of falling off sizing material increases, and the cleaning power decreases. When FMES is used alone, it can only slowly disperse the organic matter on the surface of the fabric and cannot penetrate into the interior of the glass fiber of the fabric, which is inefficient. Therefore, FMEE and FMES need to be compounded. FMEE peels off the sizing material in the interior of the glass fiber, and FMES disperses the peeled-off sizing material into the solution to prevent the re-staining of the organic matter and improve the desizing efficiency of the glass fiber organic matter. The penetrating agent is a non-ionic penetrating agent, such as fatty alcohol polyoxyethylene ether-7 and pentyl phenol polyoxyethylene ether-8, which accelerates the penetration of the liquid and promotes the rapid penetration of the desizing solution into the fiber micropores to assist the dispersion of the sizing material.

[0023] In the preparation of desizing solution, sodium percarbonate is added 20±3 min later, and then tetraacetylethylenediamine is added, so that the initial weak alkaline condition is beneficial to the decomposition of hydrogen peroxide, and the pH is lowered after the addition of tetraacetylethylenediamine, which is beneficial to the bleaching of peroxyacetic acid and the biological enzyme treatment under neutral condition. If the time is too late, the bleaching effect will be affected.

[0024] Preferably, in step S1, the CO2 pressure is 20-25 MPa, the desizing solution temperature is 52-58℃ (if the temperature is low, the enzyme activity is low, if the temperature is too high, the enzyme will be inactivated, and the hydrogen peroxide will be ineffective), and the quartz glass fiber cloth is treated in the CO2 desizing reactor for 24-26 min.

[0025] Preferably, in step S2, the water temperature in the water tank is 54-60℃, and the conveying speed of the quartz glass fiber cloth is 28-32 m / min, if the speed is too fast, the tension of the cloth will be uneven, resulting in wrinkles on the cloth surface, and the ultrasonic water washing, hydroentanglement cleaning and spraying cleaning time of the cloth is short, which cannot achieve the cleaning and fiber opening effect; the rotation speed of the wave wheel is 95-100 m / min; in step S3, the water pressure of the first water spraying hole is 2.5-4.5 kg, and the water temperature is 10-30℃; in step S4, the water pressure of the second water spraying hole is 3.5-5.5 kg, and the water temperature is 10-30℃; in step S4, the drying temperature is 59-61℃, and if the drying temperature is too high, the strength loss of the cloth surface will be large.

[0026] Compared with the prior art, the present application has the following beneficial effects:

[0027] 1. The desizing method of the present application replaces the traditional KH continuous heat treatment desizing and BH stewing secondary desizing high-temperature heat treatment mode, and adopts a more moderate mode, CO2 is combined with desizing solution, the quartz glass fiber cloth is first pre-reacted in CO2 fluid, CO2 has high permeability and dispersity, the organic matter on the surface of the quartz glass fiber cloth is pre-degraded, the directional impact on the fiber is small, the yarn bundle can be relaxed and dispersed, and the integrity of the yarn form can be ensured, which prepares for subsequent hydroentanglement. Then the organic matter is washed by ultrasonic water washing, hydroentanglement and spraying in sequence, the decomposed organic matter is removed by water washing, and the residual organic matter is continuously cleaned by hydroentanglement and spraying, and fiber opening is realized. Finally, the cloth surface is dried for FN post-treatment. The desizing method of the present application can reduce the concentration of desizing solution, reduce the desizing time and temperature, thereby reducing the energy consumption and improving the desizing effect. For the quartz glass fiber cloth product, the strength loss of the cloth surface can be reduced. Compared with the existing process, the stewing will harden the fiber and is not conducive to the fiber opening in the subsequent FN process, and the present application realizes fiber opening during the desizing process, thereby solving the problem.

[0028] 2. Traditional desizing solutions use strong alkalis and surfactants, which only cause swelling without chemical reaction, damaging the fibers and making the fabric surface rough. The sizing agent coating the surface of quartz glass fiber cloth mainly consists of starch, polyvinyl alcohol (PVA), and polyethylene glycol (PEG). The aqueous solution in the bath has high viscosity, and PVA easily forms gels, which can easily back-adhere to the fabric, forming sizing spots. For ultra-thin specialty fabrics, this can easily clog the fabric's gaps and pores. Traditional desizing solutions use highly specific enzymes and KMnO4, which has strong oxidizing properties, resulting in reduced fabric strength and easy wrinkling and pilling. The acids used can also damage the fibers. This invention utilizes a combination of compound enzymes and H2O2 oxidation to make desizing gentler. Furthermore, by adding auxiliaries, back-adhesion to the fabric is prevented. The desizing solution used in this invention contains a compound of chelating agents, penetrants, and surfactants, which work synergistically through "chelating impurities → penetrating fibers → emulsifying and dispersing" to form a highly efficient desizing system.

[0029] 3. The desizing solution of the present invention contains a pH buffer, so that the pH value is controlled at around 7, and no acid-base neutralization is required after desizing, and it can be discharged directly. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the structure of the high-efficiency desizing device for ultra-low dielectric loss electronic-grade quartz glass fiber cloth of the present invention.

[0031] Figure 2 This is a schematic diagram of the CO2 desizing reactor of the present invention.

[0032] Figure 3 This is a schematic diagram of the ultrasonic water washing tank of the present invention.

[0033] Figure 4 This is a schematic diagram of the structure of the roller of the present invention.

[0034] Figure 5 This is a schematic diagram of the hydroentangling mechanism of the present invention.

[0035] Figure 6 This is a schematic diagram of the spray mechanism of the present invention.

[0036] In the diagram, 101 is the housing; 102 is the air inlet; 103 is the air outlet; 104 is the desizing agent nozzle; 105 is the reel; 106 is the filter membrane; 107 is the flow guide horn; 2 is the ultrasonic water washing tank; 201 is the water tank; 202 is the drum; 203 is the water outlet; 204 is the ultrasonic rod; 205 is the impeller; 3 is the hydroentangling mechanism; 301 is the first water spray pipe; 302 is the first water spray hole; 4 is the spraying mechanism; 401 is the second water spray pipe; 402 is the second water spray hole; 5 is the take-up shaft; 6 is the conveyor roller; 7 is the tension roller; 8 is the pressing roller; 9 is the quartz glass fiber cloth; and 10 is the drying oven. Detailed Implementation

[0037] In order for those skilled in the art to better understand the technical solutions in the present application, the technical solutions of the present application will be clearly and completely described below in combination with embodiments of the present application.

[0038] The high-efficiency desizing device for the ultra-low dielectric loss electronic-grade quartz glass fiber cloth used in the following embodiments includes a CO2 desizing reactor, an ultrasonic water washing tank 2, a water jet mechanism 3, a spraying mechanism 4, a drying mechanism, and a winding shaft 5, as shown in the figure. Figure 1 The CO2 desizing reactor, the ultrasonic water washing tank 2, the water jet mechanism 3, the spraying mechanism 4, the drying mechanism, and the winding shaft 5 are provided with a conveying roller 6 therebetween, and the quartz glass fiber cloth 9 is conveyed through the conveying roller 6.

[0039] As shown in the figure, Figure 2 The CO2 desizing reactor includes a shell 101, the shell 101 is provided with an air inlet 102 and an air outlet 103 at two ends respectively, a filter membrane 106 is arranged at the air inlet 102, and a flow guide horn 107 is arranged at the air inlet 102 in the shell 101, so that the CO2 fluid fills the entire CO2 desizing reactor; a desizing liquid nozzle 104 is mounted at the top, a winding shaft 105 is arranged in the shell 101, and the quartz glass fiber cloth 9 is wound on the winding shaft 105.

[0040] As shown in the figure, Figure 1 , 3 The ultrasonic water washing tank 2 is provided with two, each ultrasonic water washing tank 2 includes a water tank 201, two tension rollers 7 are arranged above and below at the feeding end and the discharging end of the water tank 201 respectively, and the quartz glass fiber cloth 9 passes between the two tension rollers 7. A roller 202 is arranged in the water tank 201, and the roller 202 is driven to rotate by a motor, as shown in the figure. Figures 3-4 A water outlet hole 203 is arranged on the roller 202, the hole diameter is 5 mm, and the hole spacing is 10 mm; as shown in the figure, Figure 3 The feeding end and the discharging end of the water tank 201 are respectively provided with a pressing roller 8, so that the quartz glass fiber cloth 9 adheres to the surface of the roller 202, the quartz glass fiber cloth 9 is conveyed by rolling with the roller 202, and a ultrasonic rod 204 is arranged at the center in the roller 202; as shown in the figure, Figure 3 A plurality of wave wheels 205 are arranged in the roller 202 along the length direction of the roller 202, and the wave wheels 205 are driven to rotate by a motor.

[0041] As shown in the figure, Figure 5 The water jet mechanism 3 includes a water jet pipe one 301, the water jet pipe one 301 is provided with six rows of misaligned water jet holes one 302 at the bottom, the hole diameter is 0.1 mm, the hole spacing is 0.2 mm, the distance between the water jet holes one 302 and the quartz glass fiber cloth 9 is 8 cm; water is sprayed through the water jet holes one 302 to the quartz glass fiber cloth 9 below, to flush the residual organic matter of the quartz glass fiber cloth 9 and open the fiber. As shown in the figure, Figure 6As shown, the spraying mechanism 4 includes a water spraying pipe two 401, which is provided with a row of water spraying holes two 402 at the bottom, with a hole diameter of 0.5 mm and a hole spacing of 5 cm, and the distance between the water spraying holes two 402 and the quartz glass fiber cloth 9 is 10 cm; water is sprayed through the water spraying holes two 402 to the quartz glass fiber cloth 9 below to wash the residual organic matter of the quartz glass fiber cloth 9 and open the fiber.

[0042] As shown in Figure 1 The drying mechanism includes a drying furnace 10, and four conveying rollers 6 are arranged in the drying furnace 10. The quartz glass fiber cloth 9 is conveyed and dried in the drying furnace 10 through the conveying rollers 6.

[0043] Example 1

[0044] The efficient desizing method of the ultra-low dielectric loss electronic-grade quartz glass fiber cloth of the embodiment includes the following steps:

[0045] S1 Pre-desizing

[0046] The quartz glass fiber cloth 9 is wound on the spool 105 and placed in the CO2 desizing reactor. The desizing solution is sprayed to the quartz glass fiber cloth 9 through the desizing solution nozzle 104, and at the same time, CO2 is introduced into the CO2 desizing reactor through the gas inlet 102 and flows out through the gas outlet 103. The CO2 pressure is 20 MPa, the desizing solution temperature is 55℃, and the treatment time of the quartz glass fiber cloth 9 in the CO2 desizing reactor is 25 min.

[0047] Among them, every 1000L desizing solution includes the following mass percentage of components: sodium percarbonate 10.5%, tetraacetyl ethylenediamine 3.5%, PVA degrading enzyme Alcaligenes faecalis 0.35%, PEG degrading enzyme Bacillus 0.35%, amylase Bacillus subtilis 0.35%, pH buffer 4%, penetrating agent 1%, anti-staining agent 14.25%, and the balance is pure water. Among them, the pH buffer is sodium phosphate dibasic 3% and citric acid 1%; the anti-staining agent is octadecanoic acid polyoxybutylene-7 acetate 5.7% and octadecanoic acid polyoxybutylene-7 acetate sodium sulfonate 8.55%; the penetrating agent is fatty alcohol polyoxyethylene ether-7.

[0048] S2 Ultrasonic water washing

[0049] The spool 105 of quartz glass fiber cloth 9 wound with pre-desized quartz glass fiber cloth is taken out from the CO2 desizing reactor, and under the action of the winding shaft 5, the quartz glass fiber cloth 9 is conveyed to the ultrasonic washing tank 2 through the conveying roller 6 at a conveying speed of 32 m / min. The water temperature in the water tank 201 is 57°C, and the quartz glass fiber cloth 9 is conveyed by rolling the drum 202 under the action of the two pressing rollers 8. At the same time, the ultrasonic rod 204 emits ultrasonic waves to further clean the surface of the quartz glass fiber cloth 9 and the sizing agent contained in the quartz glass fiber yarn, thereby improving the desizing effect. At the same time, the impeller 205 pushes the water in the drum 202 to the water outlet hole 203 of the drum 202 to spray out, and the rotating speed of the impeller 205 is 95 m / min, which can flush away the organic residues on the surface of the quartz glass fiber cloth 9 wound on the drum 202.

[0050] S3 water jet

[0051] After ultrasonic water washing, the quartz glass fiber cloth 9 is conveyed to the water jet mechanism 3 through the conveying roller 6, and water is sprayed on the quartz glass fiber cloth 9 through the water spraying pipe one 301, the water pressure is 3.5 kg, the water temperature is 20°C, the residual organic matter of the quartz glass fiber cloth 9 is washed and opened, and the width of the warp yarn is opened, thereby reducing the air permeability of the cloth and preparing for further post-processing.

[0052] S4 spraying

[0053] After water jetting, the quartz glass fiber cloth 9 is conveyed to the spraying mechanism 4 through the conveying roller 6, and water is sprayed on the quartz glass fiber cloth 9 through the water spraying pipe two 401, the water pressure is 4.5 kg, the water temperature is 20°C, the residual organic matter of the quartz glass fiber cloth 9 is further washed and opened, and the width of the weft yarn is opened, thereby reducing the air permeability of the cloth and preparing for further post-processing.

[0054] S5 drying: the quartz glass fiber cloth 9 after spraying is conveyed to the drying mechanism through the conveying roller 6, and is dried at 60°C.

[0055] S6 winding: the quartz glass fiber cloth 9 after drying is wound on the winding shaft 5.

[0056] Example 2

[0057] The efficient desizing method of the ultra-low dielectric loss electronic grade quartz glass fiber cloth of the present embodiment comprises the following steps:

[0058] S1 pre-desizing

[0059] The quartz glass fiber cloth 9 is wound on the winding shaft and put into the CO2 desizing reactor. The desizing solution is sprayed to the quartz glass fiber cloth 9 through the desizing solution nozzle 104, and at the same time, the CO2 is introduced into the CO2 desizing reactor through the gas inlet 102 and flows out through the gas outlet 103. The CO2 pressure is 25 MPa, the desizing solution temperature is 52℃, and the treatment time of the quartz glass fiber cloth 9 in the CO2 desizing reactor is 24 min.

[0060] The desizing solution includes the following components by mass percentage per 1000L: sodium percarbonate 6.25%, tetraacetyl ethylenediamine 2.5%, PVA degrading enzyme of M. esterophilus 0.5%, PEG degrading enzyme of Achromobacter 0.5%, amylase of B. licheniformis 0.5%, pH buffer 4.41%, penetrating agent 0.5%, anti-staining agent 21%, and the balance is pure water. The pH buffer is disodium hydrogen phosphate 3.36% and citric acid 1.05%; the anti-staining agent is hexadecanoic acid polyoxybutylene-7 acetate 6% and hexadecanoic acid polyoxybutylene-7 acetate sodium sulfonate 15%; and the penetrating agent is amyl phenol polyoxyethylene ether-8.

[0061] S2 ultrasonic water washing

[0062] The same as example 1, except that the water temperature of the ultrasonic water washing tank 2 is 54℃, and the conveying speed of the quartz glass fiber cloth 9 is 30 m / min.

[0063] S3 water jet

[0064] The quartz glass fiber cloth 9 after ultrasonic water washing is conveyed to the water jet mechanism 3 through the conveying roller 6, and water is sprayed to the quartz glass fiber cloth 9 through the water jet pipe one 301, the water pressure is 2.5 kg, and the water temperature is 10℃. The residual organic matter of the quartz glass fiber cloth 9 is washed and opened, and the width of the warp yarn is opened, the air permeability of the cloth is reduced, and the preparation for further post-processing is made.

[0065] S4 spraying

[0066] The quartz glass fiber cloth 9 after water jet is conveyed to the spraying mechanism 4 through the conveying roller 6, and water is sprayed to the quartz glass fiber cloth 9 through the water jet pipe two 401, the water pressure is 3.5 kg, and the water temperature is 10℃. The residual organic matter of the quartz glass fiber cloth 9 is further washed and opened, and the width of the weft yarn is opened, the air permeability of the cloth is reduced, and the preparation for further post-processing is made.

[0067] S5 drying: the quartz glass fiber cloth 9 after spraying is conveyed to the drying mechanism through the conveying roller 6, and dried at 59℃.

[0068] S6 winding: the quartz glass fiber cloth 9 after drying is wound on the winding shaft 5.

[0069] Example 3

[0070] The high-efficiency desizing method of the ultra-low dielectric loss electronic-grade quartz glass fiber cloth of the embodiment comprises the following steps:

[0071] S1 Pre-desizing

[0072] The quartz glass fiber cloth 9 is wound on the winding shaft and put into the CO2 desizing reactor. The desizing solution is sprayed to the quartz glass fiber cloth 9 through the desizing solution nozzle 104, and at the same time, CO2 is introduced into the CO2 desizing reactor through the gas inlet 102 and flows out through the gas outlet 103. The CO2 pressure is 24 MPa, the temperature is 58℃, and the treatment time of the quartz glass fiber cloth 9 in the CO2 desizing reactor is 26 min.

[0073] Among them, every 1000L desizing solution includes the following mass percentage of components: sodium percarbonate 7.5%, tetraacetyl ethylenediamine 3%, PVA degrading enzyme Alcaligenes faecalis 0.5%, PEG degrading enzyme Bacillus 0.5%, amylase Bacillus amyloliquefaciens 0.75%, pH buffer 3.61%, penetrant 1.5%, anti-staining agent 18%, and the balance is pure water. Among them, the pH buffer is disodium hydrogen phosphate 2.66% and citric acid 0.95%; the anti-staining agent is hexadecanoic acid polyoxybutylene-7 acetate 6% and hexadecanoic acid polyoxybutylene-7 acetate sodium sulfonate 12%; the penetrant is amyl phenol polyoxyethylene ether-8.

[0074] S2 Ultrasonic water washing

[0075] The same as example 1, except that the water temperature of the ultrasonic water washing tank 2 is 60℃, and the conveying speed of the quartz glass fiber cloth 9 is 28 m / min.

[0076] S3 Water jet

[0077] The quartz glass fiber cloth 9 after ultrasonic water washing is conveyed to the water jet mechanism 3 through the conveying roller 6, and water is sprayed to the quartz glass fiber cloth 9 through the water jet pipe one 301, the water pressure is 4.5 kg, and the water temperature is 30℃. The residual organic matter of the quartz glass fiber cloth 9 is washed and opened, and the width of the warp yarn can be opened, reducing the air permeability of the cloth and preparing for further post-processing.

[0078] S4 Spraying

[0079] The quartz glass fiber cloth 9 after water jet is conveyed to the spraying mechanism 4 through the conveying roller 6, and water is sprayed to the quartz glass fiber cloth 9 through the water jet pipe two 401, the water pressure is 5.5 kg, and the water temperature is 30℃. The residual organic matter of the quartz glass fiber cloth 9 is further washed and opened, and the width of the weft yarn can be opened, reducing the air permeability of the cloth and preparing for further post-processing.

[0080] S5 Drying: The quartz glass fiber cloth 9 after spraying is conveyed to the drying mechanism through the conveying roller 6 and dried at 61℃.

[0081] S6 winding: the dried quartz glass fiber cloth 9 is wound on the winding shaft 5.

[0082] Comparative Example 1

[0083] Comparative Example 1 uses the existing KH+BH process to desize the quartz glass fiber cloth 9, KH: the quartz glass fiber cloth 9 is desized at a speed of 60 m / min and passes through a furnace zone at 310℃, and the cloth is rolled in the furnace zone for 10s. BH: the whole roll of quartz glass fiber cloth 9 is burned in the furnace, which is divided into two stages, burned at 280℃ for 5h, then heated to 400℃, and burned for 35h at a heating rate of 15℃ / h.

[0084] Comparative Example 2

[0085] The difference from Example 1 is that water is used instead of the desizing solution in Example 1.

[0086] Comparative Example 3

[0087] The difference from Example 1 is that in the stain-proofing agent of the desizing solution, octadecan fatty acid polyoxybutylene-7 acetate is used instead of octadecan fatty acid polyoxybutylene-7 acetate sodium sulfonate.

[0088] Comparative Example 4

[0089] The difference from Example 1 is that in the stain-proofing agent of the desizing solution, octadecan fatty acid polyoxybutylene-7 acetate sodium sulfonate is used instead of octadecan fatty acid polyoxybutylene-7 acetate.

[0090] Comparative Example 5

[0091] The difference from Example 1 is that in step S1, no CO2 is introduced into the CO2 desizing reactor.

[0092] Comparative Example 6

[0093] The difference from Example 1 is that in step S1, the temperature of the desizing solution sprayed in the CO2 desizing reactor is 80℃.

[0094] Comparative Example 7

[0095] The difference from Example 1 is that in step S2, the ultrasonic rod 204 in the ultrasonic washing tank 2 is turned off.

[0096] The quartz glass fiber cloth 9 treated in Examples 1-3 and Comparative Examples 1-7 is tested for performance, and the test method for combustible content is as follows:

[0097] Take the desizing treated quartz glass fiber cloth 95-10 g, place it in a drying oven at 125℃ and dry for 60 min until the weight is constant; then heat it at 625℃ for 40 min until the weight is constant, and the combustible content (%) = the weight loss of the sample after heating to constant weight / the weight of the sample after heating to constant weight.

[0098] The tensile breaking strength of the coated glass fiber yarn was tested using a tensile testing machine.

[0099] The warp and weft yarn widths were measured using a microscope.

[0100] The test results are shown in Table 1:

[0101] Table 1: Performance test results of the treated quartz glass fiber cloth 9 of Examples 1-3 and Comparative Examples 1-7

[0102]

[0103]

[0104] In Comparative Example 1, high-temperature heat desizing was used, which damaged the surface structure of the quartz glass fiber cloth 9, resulting in a decrease in tensile breaking strength; during the whole cloth braising, the temperature was unevenly heated and contacted with air, resulting in a high combustible content; and the yarns hardened after braising, which was not conducive to the FN opening process in the subsequent process, resulting in a narrow warp and weft yarn width.

[0105] In Comparative Example 2, water was used as the desizing solution, which could not degrade the organic matter in the quartz glass fiber cloth 9, resulting in a high combustible content; the high combustible content also resulted in less coupling agent coating in the subsequent FN process, less strength recovery on the cloth surface, and finally a decrease in tensile breaking strength.

[0106] In Comparative Example 3, sodium octadecyl fatty acid polyoxybutylene-7 acetate sulfonate was not used in the desizing solution, which caused the detached organic matter to re-contaminate and could not effectively degrade the organic matter, resulting in a high combustible content on the cloth surface, which in turn led to less coupling agent coating in the subsequent FN process, less strength recovery on the cloth surface, and a decrease in tensile breaking strength.

[0107] In Comparative Example 4, octadecyl fatty acid polyoxybutylene-7 acetate was not used in the desizing solution, which caused the desizing solution to fail to fully penetrate into the glass fiber inside and could not effectively degrade the organic matter in a short time, resulting in a high combustible content on the cloth surface, which in turn led to less coupling agent coating in the subsequent FN process, less strength recovery on the cloth surface, and a decrease in tensile breaking strength.

[0108] In Comparative Example 5, CO2 was not introduced into the CO2 desizing reactor, which could not make the desizing solution fully react with the organic matter on the surface of the glass fiber cloth in a short time, resulting in a high combustible content on the cloth surface, which in turn led to less coupling agent coating in the subsequent FN process, less strength recovery on the cloth surface, and a decrease in tensile breaking strength.

[0109] The temperature of the desizing solution used in Comparative Example 6 was too high, which caused ineffective decomposition of hydrogen peroxide, reduced enzyme activity, and ineffective degradation of organic matter, resulting in a high content of combustible matter on the fabric surface, which in turn led to less coupling agent coated in the FN process, less strength recovery of the fabric surface, and reduced tensile breaking strength.

[0110] In Comparative Example 7, no ultrasonic was used during washing, which could not effectively separate the organic matter on the fabric surface, resulting in a high content of combustible matter on the fabric surface, which in turn led to less coupling agent coated in the FN process, less strength recovery of the fabric surface, and reduced tensile breaking strength.

Claims

1. An efficient desizing device for ultra-low dielectric loss electronic-grade quartz glass fiber cloth, characterized in that it comprises a CO2 desizing reactor, an ultrasonic water washing tank (2), a water jet mechanism (3), a spraying mechanism (4), a drying mechanism and a winding shaft (5), the ultrasonic water washing tank (2), the water jet mechanism (3), the spraying mechanism (4), the drying mechanism and the winding shaft (5) are provided with conveying rollers (6) therebetween, and the quartz glass fiber cloth (9) is conveyed through the conveying rollers (6). The CO2 desizing reactor comprises a shell (101), the two ends of the shell (101) are respectively provided with an air inlet (102) and an air outlet (103), a desizing liquid nozzle (104) is mounted on the top, a winding shaft (105) is arranged in the shell (101), and the quartz glass fiber cloth (9) is wound on the winding shaft (105). The ultrasonic water washing tank (2) comprises a water tank (201), a roller (202) is arranged in the water tank (201), the roller (202) is driven to rotate by a motor, water outlets (203) are arranged on the roller (202), the quartz glass fiber cloth (9) is attached to the surface of the roller (202), the quartz glass fiber cloth (9) is conveyed by rolling with the roller (202), and an ultrasonic rod (204) is arranged at the center of the roller (202). The water jet mechanism (3) comprises a water jet pipe I (301), a plurality of water jet holes I (302) are arranged at the bottom of the water jet pipe I (301) to spray water on the quartz glass fiber cloth (9) below, wash the residual organic matter of the quartz glass fiber cloth (9) and open the fiber. The spraying mechanism (4) comprises a water jet pipe II (401), a water jet hole II (402) is arranged at the bottom of the water jet pipe II (401) to spray water on the quartz glass fiber cloth (9) below, wash the residual organic matter of the quartz glass fiber cloth (9) and open the fiber. The air inlet (102) of the CO2 desizing reactor is provided with a filter membrane (106), and a flow guide horn (107) is arranged at the air inlet (102) in the shell (101).

2. The efficient desizing device of ultra-low dielectric loss electronic grade quartz glass fiber cloth (9) according to claim 1, characterized in that, A plurality of wave wheels (205) are arranged in the roller (202) along the length direction of the roller (202), the wave wheels (205) are driven to rotate by a motor, the water outlets (203) on the roller (202) have a hole diameter of 2-5 mm and a hole spacing of 5-10 mm, two tension rollers (7) are arranged above and below the feeding end and the discharging end of the ultrasonic water washing tank (2) respectively, the quartz glass fiber cloth (9) passes between the two tension rollers (7), and the feeding end and the discharging end of the ultrasonic water washing tank (2) are respectively provided with pressing rollers (8) to make the quartz glass fiber cloth (9) adhere to the surface of the roller (202).

3. The efficient desizing device of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 1, characterized in that, The drying mechanism comprises a drying furnace (10), a plurality of conveying rollers (6) are arranged in the drying furnace (10), and the quartz glass fiber cloth (9) is conveyed and dried in the drying furnace (10) through the conveying rollers (6).

4. The efficient desizing device of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 1, characterized in that, ​ 5. The efficient desizing device of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 1, characterized in that, The bottom of the water spraying pipe one (301) is provided with six rows of water spraying holes one (302) with a hole diameter of 0.05-0.1 mm and a hole spacing of 0.1-0.2 mm, and the distance between the water spraying holes one (302) and the quartz glass fiber cloth (9) is 7-9 cm; the bottom of the water spraying pipe two (401) is provided with one row of water spraying holes two (402) with a hole diameter of 0.4-0.5 mm and a hole spacing of 5-8 cm, and the distance between the water spraying holes two (402) and the quartz glass fiber cloth (9) is 9-11 cm.

6. A high efficiency desizing process for ultra-low dielectric loss electronic grade quartz glass fiber cloth, characterized by, The efficient desizing of the ultra-low dielectric loss electronic-grade quartz glass fiber cloth is carried out by the efficient desizing device of the ultra-low dielectric loss electronic-grade quartz glass fiber cloth according to any one of claims 1-5, including the following steps: S1, pre-desizing: the quartz glass fiber cloth (9) wound on the winding shaft (105) is placed in the CO2 desizing reactor, the desizing liquid is sprayed to the quartz glass fiber cloth (9) through the desizing liquid nozzle (104), and the CO2 is introduced into the CO2 desizing reactor through the gas inlet (102) and flows out through the gas outlet (103); during the process, the sizing on the surface of the quartz glass fiber cloth (9) reacts with the desizing liquid and is carried away by the CO2 flow, realizing the pre-desizing of the sizing on the surface of the quartz glass fiber cloth (9); S2, ultrasonic water washing: the winding shaft (105) with the pre-desized quartz glass fiber cloth (9) is taken out of the CO2 desizing reactor, under the action of the winding shaft (5), the quartz glass fiber cloth (9) is conveyed to the ultrasonic water washing tank (2) through the conveying roller (6) and is attached to the surface of the roller (202), the quartz glass fiber cloth (9) is conveyed by rolling the roller (202), and at the same time, the ultrasonic waves emitted by the ultrasonic rod (204) further clean the sizing on the surface of the quartz glass fiber cloth (9) and the quartz glass fiber, improving the desizing effect; S3, water jet: the quartz glass fiber cloth (9) after ultrasonic water washing is conveyed to the water jet mechanism (3) through the conveying roller (6), the quartz glass fiber cloth (9) is sprayed by the water spraying pipe one (301), and the residual organic matter of the quartz glass fiber cloth (9) is washed and fibrillated; S4, spraying: the quartz glass fiber cloth (9) after water jet is conveyed to the spraying mechanism (4) through the conveying roller (6), the quartz glass fiber cloth (9) is sprayed by the water spraying pipe two (401), and the residual organic matter of the quartz glass fiber cloth (9) is further washed and fibrillated; S5, drying: the quartz glass fiber cloth (9) after spraying is conveyed to the drying mechanism for drying through the conveying roller (6); S6, winding: the quartz glass fiber cloth (9) after drying is wound on the winding shaft (5).

7. The efficient desizing method of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 6, characterized in that, In step S1, 1000L of the desizing solution comprises the following components in percentage by mass: sodium percarbonate 6.25-10.5%, tetraacetylethylenediamine 2.5-3.5%, PVA-degrading enzyme 0.35-0.5%, PEG-degrading enzyme 0.35-0.5%, amylase 0.35-0.75%, pH buffer 3.61-4.41%, penetrating agent 0.5-1.5%, anti-staining agent 14.25-21%, and the balance being pure water; wherein the pH buffer is disodium hydrogen phosphate 2.66-3.36% and citric acid 0.95-1.05%, and the anti-staining agent is 5.7-6% FMEE and 8.55-15% FMES.

8. The efficient desizing method of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 7, characterized in that, The mass ratio of sodium percarbonate to tetraacetylethylenediamine is (2.5-3):1; in the pH buffer, the mass ratio of disodium hydrogen phosphate to citric acid is (2.8-3.2):1; the mass ratio of PVA-degrading enzyme, PEG-degrading enzyme and amylase is 1:1:(1-1.5); in the anti-staining agent, the mass ratio of FMEE to FMES is 1:(1.5-2.5); and the penetrating agent is a non-ionic penetrating agent.

9. The efficient desizing method of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 6, characterized in that, In step S1, the CO2 pressure is 20-25MPa, the temperature of the desizing solution is 52-58℃, and the treatment time of the quartz glass fiber cloth (9) in the CO2 desizing reactor is 24-26min.

10. The efficient desizing method of ultra-low dielectric loss electronic grade quartz glass fiber cloth according to claim 6, characterized in that, In step S2, the water temperature in the water tank (201) is 54-60℃, the conveying speed of the quartz glass fiber cloth (9) is 28-32m / min, and the rotation speed of the impeller (205) is 95-100m / min; in step S3, the water pressure of the water spraying hole one (302) is 2.5-4.5kg, and the water temperature is 10-30℃; in step S4, the water pressure of the water spraying hole two (402) is 3.5-5.5kg, and the water temperature is 10-30℃; and in step S4, the drying temperature is 59-61℃.

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