CN114645365A - Splitting process easy to clean electronic-grade glass fiber cloth slurry and slurry used in splitting process - Google Patents

Splitting process easy to clean electronic-grade glass fiber cloth slurry and slurry used in splitting process Download PDF

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Publication number
CN114645365A
CN114645365A CN202210278895.XA CN202210278895A CN114645365A CN 114645365 A CN114645365 A CN 114645365A CN 202210278895 A CN202210278895 A CN 202210278895A CN 114645365 A CN114645365 A CN 114645365A
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temperature
slurry
electronic
glass fiber
grade glass
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Inventor
刘东锋
李冲
褚富裕
李伟
李洲
康凤楠
肖华青
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Taishan Fiberglass Zoucheng Co Ltd
China National Building Material Group Co Ltd CNBM
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Taishan Fiberglass Zoucheng Co Ltd
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Priority to CN202210278895.XA priority Critical patent/CN114645365A/en
Publication of CN114645365A publication Critical patent/CN114645365A/en
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    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/242Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads inorganic, e.g. basalt
    • D03D15/267Glass
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D1/00Woven fabrics designed to make specified articles
    • D03D1/0088Fabrics having an electronic function
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B15/00Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/04Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of yarns, threads or filaments
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/10Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/144Alcohols; Metal alcoholates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/327Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
    • D06M15/333Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)

Abstract

The invention belongs to the technical field of preparation of electronic-grade glass fiber cloth, and particularly relates to a fiber splitting process easy for cleaning slurry of the electronic-grade glass fiber cloth and the slurry used by the same. The splitting process easy to clean the slurry of the electronic-grade glass fiber cloth comprises the following steps of: size preparation → warping slashing → weaving gray fabric → fiber opening of gray fabric → BH smoldering (batch heat treatment) → FN surface treatment (surface chemical treatment). The invention provides the slurry which is easy to clean, has good removal effect, saves energy and reduces consumption in the application of preparing electronic-grade glass fiber cloth, and can ensure the strength and impregnation performance of the electronic cloth.

Description

Splitting process easy to clean electronic-grade glass fiber cloth slurry and slurry used in splitting process
Technical Field
The invention belongs to the technical field of preparation of electronic-grade glass fiber cloth, and particularly relates to a fiber splitting process easy for cleaning slurry of the electronic-grade glass fiber cloth and the slurry used by the same.
Background
The traditional electronic cloth sizing agent can achieve excellent coating performance on yarns at present, the weaving performance basically meets the requirements of the existing industry, but high-temperature desizing is needed in the production process, a large amount of energy is consumed in the process, and the increase of production cost and the waste of energy are caused. In addition, along with the trend of thinning electronic cloth, the surface treatment process of the thin electronic cloth is also changed, and is different from the traditional electronic cloth surface treatment process, the thin electronic cloth is not generally subjected to one-time desizing, namely continuous desizing, about 90% of slurry is removed by using high temperature of about 400 ℃, but the gray cloth is subjected to one-time desizing by adopting fiber opening of gray cloth, but the gray cloth produced by the method has more residual slurry on the surface than the continuous desizing, so that the impregnation property and the physical property of a product are adversely affected, in order to fully remove the slurry, the BH stewing time needs to be prolonged, glass fiber is greatly damaged, the strength of the electronic cloth is reduced, and aiming at the phenomenon, the prior art proposes that alpha-starch desizing enzyme is added into a hot water tank of a gray cloth fiber opener to improve the removal effect of the slurry, but the implementation process of the technology is to keep the activity of the alpha-starch desizing enzyme, the water temperature of the hot water tank needs to be controlled between 60 ℃ and 95 ℃, and the energy waste problem exists.
CN200910056345.8 discloses an electronic grade glass fiber cloth fiber-opening process and slurry thereof, the process comprises the steps of firstly preparing the slurry and boiling the slurry, adding water into polyvinyl alcohol of the main slurry, stirring and heating to dissolve, adding a leavening agent quaternary ammonium salt type surfactant after the polyvinyl alcohol is completely dissolved and becomes transparent and clear solution, and dissolving for use; 5-10% of main pulp polyvinyl alcohol, and 0.5-1% of cationic surfactant as a swelling agent; then slashing for subsequent weaving into grey cloth; performing high-temperature combustion desizing on the woven electronic-grade glass fiber cloth gray cloth for the first time, and then intensively putting the gray cloth into a furnace for long-time smoldering desizing; and finishing the treatment of coating the silane coupling agent on the surface of the glass fiber cloth after the two desizing treatments. And the residual size of the grey cloth caused by the one-time high-temperature desizing is large.
CN201711109279.7 discloses a novel sizing process of polyvinyl alcohol-free size, which comprises the steps of treating a textile by plasma, adding the polyvinyl alcohol-free size for sizing, desizing by plasma treatment, and recycling the obtained desized liquid in the sizing process of the polyvinyl alcohol-free size after the textile is treated by the plasma; or adding the textile into the sizing agent containing the polyvinyl alcohol for sizing, then carrying out plasma treatment for desizing, and recycling the obtained desizing liquid in the sizing process containing the polyvinyl alcohol sizing agent, thereby realizing the purposes of energy conservation and emission reduction. Such plasma desizing is less effective.
CN201810826137.0 discloses an electronic-grade glass fiber cloth blank fabric opening method, which is to add alpha-starch desizing enzyme into a hot water tank, control the water temperature at 60-95 ℃, and ensure the enzyme activity of the alpha-starch desizing enzyme to be: 8500-9300U/mL, pH value: 5.4-6.4, density: 1.1-1.2 g/cm; enabling the electronic-grade glass fiber cloth blank cloth to pass through a hot water tank, and soaking for 3-5 seconds in the hot water tank; and opening the soaked grey cloth. The problem of high residual pulp rate on the surface of the blank opening cloth produced by a grey cloth opening mode is solved, but the resource waste is serious.
Disclosure of Invention
The invention aims to provide the slurry which is easy to clean, has good removal effect, saves energy and reduces consumption in the application of preparing electronic-grade glass fiber cloth, and can ensure the strength and impregnation performance of the electronic cloth.
The invention relates to a fiber splitting process easy for cleaning electronic grade glass fiber cloth slurry, which comprises the following steps: size preparation → warping slashing → weaving gray fabric → fiber opening of gray fabric → BH smoldering (batch heat treatment) → FN surface treatment (surface chemical treatment).
The slurry preparation steps comprise:
(1) adding pure water into the liquid preparation cylinder, starting the stirrer, and setting the frequency to be 43-50 HZ;
(2) adding polyvinyl alcohol for 3-10min, circulating for 2-3min, reducing stirring frequency to 30-35HZ, heating to 85-95 deg.C, maintaining for 20-25min, and maintaining for 30-40 min;
(3) cooling to 40-50 ℃, adding the assistant A, the assistant B and the balance of pure water, and continuing stirring for later use.
The operating speed of the warping slasher is 60-180 m/min; the curling tension is 10-20N; the grouting pressure is 0.4-0.5 Mpa; the temperature of the pulp tank is 40-50 ℃; the oven temperature was 100-130 ℃.
The running speed of a weaving machine for weaving the gray fabric is 500-700rpm, and the let-off tension is 80-350N; the TW angle was 225-240 °; the main spray pressure is 1.0-3.5 kgf.
The running speed of a grey cloth splitting machine is 15-30 m/min; the rotating speed of the roller is 200-500 rpm; the temperature of the hot water tank is 40-50 ℃; the drying temperature is 55-65 ℃.
The BH smoldering stage is divided into four temperature rising stages: the first stage is to raise the room temperature to 260-270 ℃ for 400-540 min; the second stage is a keeping stage, the temperature is kept at 260-270 ℃ and the time is kept at 660-780 min; the third stage is that the temperature is increased from 260 ℃ to 380 ℃ and 390 ℃ for 240 ℃ and 360 min; the second stage is a maintaining stage, wherein the temperature is maintained at 380-.
The running speed of the FN surface treatment machine is 50-80 m/min; the sending tension is 100-160N; the curling tension is 120-220N; the drying temperature is 105-125 ℃.
The slurry easy to clean the electronic grade glass fiber cloth slurry is prepared from the following raw materials in percentage by mass:
Figure BDA0003553742230000021
the alcoholysis degree dB of polyvinyl alcohol (PVA) is 78-82%, the polymerization degree n is 300-400, and the polyvinyl alcohol is preferably PVA 3-80;
the auxiliary agent A is fatty alcohol-polyoxyethylene ether, preferably PVA 5-88;
the auxiliary agent B is micromolecular alcohol, and the micromolecular alcohol is methanol and ethanol.
Specifically, the splitting process easy for cleaning the slurry of the electronic-grade glass fiber cloth comprises the following steps of:
(1) preparation of slurry
a. Adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43-50 HZ;
b. adding the auxiliary agent A and the auxiliary agent B in the formula amount, and continuously stirring;
c. slowly adding the formula amount of raw material polyvinyl alcohol for 3-10min, starting a circulating pump, circulating for about 2-3min, setting the temperature to 85-95 ℃ after the addition is finished, reducing the stirring frequency to 30-35HZ, slowly heating, controlling the heating time to 20-25min, setting the temperature to 85-95 ℃, keeping the temperature for 30-40min, and uniformly stirring;
d. adding the balance of pure water to 1000L, assisting to cool, cooling to the set value of 40-50 ℃, and keeping for later use;
(2) warping slashing
The operating speed of the warping slasher is 60-180 m/min; the curling tension is 10-20N; the grouting pressure is 0.4-0.5 Mpa; the temperature of the pulp tank is 40-50 ℃; the temperature of the oven is 100-130 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving the gray fabric is 500-700rpm, and the let-off tension is 80-350N; the TW angle was 225-240 °; the main spraying pressure is 1.0-3.5 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 15-30 m/min; the rotating speed of the roller is 200-500 rpm; the temperature of the hot water tank is 40-50 ℃; the drying temperature is 55-65 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 260-270 400-540
2 260-270 260-270 660-780
3 260-270 380-390 240-360
4 380-390 380-390 960-1080
(6) FN surface treatment
The running speed of the FN surface treatment machine is 50-80 m/min; the sending tension is 100-160N; the curling tension is 120-220N; the drying temperature is 105-125 ℃.
The slurry used in the fiber opening process for easily cleaning the slurry of the electronic-grade glass fiber cloth is prepared by cleaning the slurry of the electronic-grade glass fiber cloth, which is easy to be cleaned by using polyvinyl alcohol as a main slurry, polyvinyl alcohol with 78-82% of alcoholysis degree dB and 300-400 of polymerization degree n, a synergistic agent A and an auxiliary agent B, in a warm water state at 40-50 ℃ while meeting the weaving requirement, and by using a staged BH temperature rise curve in combination with the thermal decomposition property of polyvinyl alcohol PVA3-80, the removal effect of the slurry is ensured, the damage of the glass fiber is reduced, and the strength of the glass cloth is improved; the combined sizing agent is quickly dissolved at low temperature, the warping weaving production requirement is guaranteed, meanwhile, the residual amount of sizing agent of the grey cloth splitting fabric is reduced by matching with a grey cloth splitting machine process, the BH stewing time is reduced, and the strength and the impregnation performance of the electronic cloth are guaranteed.
Compared with the prior art, the invention has the following beneficial effects:
(1) by adopting the splitting process for cleaning the electronic-grade glass fiber cloth slurry, the removal of the slurry reaches 83 percent, the removal effect is good, and the soaking of the glass cloth and the resin is facilitated;
(2) by adopting the splitting process for cleaning the slurry of the electronic-grade glass fiber cloth, the BH smoldering time is reduced, the damage of glass fibers is reduced, and the strength of the electronic-grade glass fiber cloth is improved;
(3) by adopting the opening process for cleaning the electronic-grade glass fiber cloth sizing agent, the residual amount of the sizing agent of the grey cloth opening cloth is reduced, and the energy is saved and the consumption is reduced.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
The specification of the easy electronic grade glass fiber cloth is 1080, and the slurry cleaning fiber opening process comprises the following steps:
a. adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43 HZ;
b. slowly adding 5.0% PVA3-80 by mass ratio for 3min, opening a circulating pump, circulating for about 2min, setting the temperature to 85 ℃ after the addition is finished, reducing the stirring frequency to 30HZ, slowly heating, controlling the heating time to 20min, setting the temperature to 85 ℃, keeping the temperature for 30min, and stirring at constant speed;
c. adding pure water for auxiliary cooling, and cooling to a set value of 40 ℃;
d. adding 0.1 percent of fatty alcohol-polyoxyethylene ether, 0.1 percent of methanol and the balance of pure water by mass percent to 1000L, and continuously stirring for later use.
(2) Warping slashing
The operating speed of the warping slasher is 180 m/min; the crimp tension was 20N; the grouting pressure is 0.5 Mpa; the temperature of the slurry tank is 40 ℃; the oven temperature is 130 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving the grey cloth is 700rpm, and the let-off tension is 350N; the TW angle is 240 °; the main spraying pressure is 3.5 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 30 m/min; the rotating speed of the roller is 500 rpm; the temperature of the hot water tank is 40 ℃; the drying temperature is 65 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 270 540
2 270 270 780
3 270 390 360
4 390 390 1080
(6) FN surface treatment
The running speed of the FN surface treatment machine is 80 m/min; the sending tension is 160N; the crimp tension was 220N; the drying temperature is 125 ℃.
Example 2
The specification of the easy electronic grade glass fiber cloth is 1067, and the slurry cleaning fiber opening process comprises the following steps:
(1) preparation of slurry
a. Adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 45 HZ;
b. slowly adding PVA3-80 with a mass ratio of 7.0%, adding for 5min, opening a circulating pump, circulating for about 2min, setting the temperature to 90 ℃ after adding, reducing the stirring frequency to 32HZ, slowly heating, controlling the heating time to 22min, setting the temperature to 90 ℃, keeping the temperature for 35min, and stirring at a constant speed;
c. adding pure water for auxiliary cooling, and cooling to a set value of 45 ℃;
d. adding 0.4 percent of fatty alcohol-polyoxyethylene ether, 0.4 percent of ethanol and the balance of pure water by mass percent to 1000L, and continuously stirring for standby.
(2) Warping slashing
The operating speed of the warping slasher is 100 m/min; the crimp tension was 15N; the grouting pressure is 0.45 Mpa; the temperature of the slurry tank is 45 ℃; the temperature of the oven is 120 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving the grey cloth is 600rpm, and the let-off tension is 170N; the TW angle is 235 °; the main spraying pressure is 2.0 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 25 m/min; the rotating speed of the roller is 350 rpm; the temperature of the hot water tank is 45 ℃; the drying temperature is 60 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 265 480
2 265 265 720
3 265 382 300
4 382 382 1020
(6) FN surface treatment
The running speed of the FN surface treatment machine is 65 m/min; the sending tension is 130N; the crimp tension was 170N; the drying temperature is 110 ℃.
Example 3
The specification of the glass fiber cloth easy to be cleaned by electronic grade is 1027, and the fiber opening process for cleaning slurry comprises the following steps:
(1) preparation of slurry
a. Adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43-50 HZ;
b. slowly adding 9.0% PVA3-80 by mass ratio for 10min, opening a circulating pump, circulating for about 3min, setting the temperature to 95 ℃ after the addition is finished, reducing the stirring frequency to 35HZ, slowly heating, controlling the heating time to 25min, setting the temperature to 95 ℃, keeping the temperature for 40min, and stirring at constant speed;
c. adding pure water for auxiliary cooling, and cooling to a set value of 50 ℃;
d. adding 1.0 percent by mass of fatty alcohol-polyoxyethylene ether, 1.0 percent by mass of ethanol and the balance of pure water to 1000L, and continuously stirring for later use.
(2) Warping slashing
The operating speed of the warping slasher is 60 m/min; the crimp tension was 10N; the grouting pressure is 0.4 Mpa; the temperature of the pulp tank is 50 ℃; the temperature of the oven is 100 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving the grey cloth is 500rpm, and the let-off tension is 80N; TW angle is 225 °; the main spraying pressure is 1.0 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 15 m/min; the rotating speed of the roller is 200 rpm; the temperature of the hot water tank is 50 ℃; the drying temperature is 55 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 260 400
2 260 260 660
3 260 380 240
4 380 380 960
(6) FN surface treatment
The running speed of the FN surface treatment machine is 50 m/min; the sending tension is 100N; the crimp tension was 120N; the drying temperature was 105 ℃.
Comparative example 1
An opening process of electronic-grade glass fiber cloth, which uses the specification of 1080 of the electronic-grade glass fiber cloth, comprises the following steps:
(1) preparation of slurry
a. Adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43 HZ;
b. slowly adding 5.0% PVA5-88 in a mass ratio for 3min, opening a circulating pump, circulating for about 2min, setting the temperature to 85 ℃ after the addition is finished, reducing the stirring frequency to 30HZ, slowly heating, controlling the heating time to 20min, setting the temperature to 85 ℃, keeping the temperature for 30min, and stirring at a constant speed; wherein the alcoholysis degree dB of the PVA5-88 is 87% -89%, and the polymerization degree n is 500-600;
c. adding pure water for auxiliary cooling, and cooling to a set value of 40 ℃;
d. adding 0.1 percent of fatty alcohol-polyoxyethylene ether, 0.1 percent of methanol and the balance of pure water by mass percent to 1000L, and continuously stirring for later use.
(2) Warping slashing
The operating speed of the warping slasher is 180 m/min; the crimp tension was 20N; the grouting pressure is 0.5 Mpa; the temperature of the slurry tank is 40 ℃; the oven temperature is 130 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving grey cloth is 700rpm, and the let-off tension is 350N; the TW angle is 240 °; the main spraying pressure is 3.5 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 30 m/min; the rotating speed of the roller is 500 rpm; the temperature of the hot water tank is 40 ℃; the drying temperature is 65 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 270 540
2 270 270 780
3 270 390 360
4 390 390 1080
(6) FN surface treatment
The running speed of the FN surface treatment machine is 80 m/min; the sending tension is 160N; the crimp tension was 220N; the drying temperature was 125 ℃.
Comparative example 2
An opening process of electronic-grade glass fiber cloth, which uses the specification of 1080 of the electronic-grade glass fiber cloth, comprises the following steps:
(1) preparation of slurry
a. Adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43 HZ;
b. slowly adding 5.0% PVA5-88 in a mass ratio for 3min, opening a circulating pump, circulating for about 2min, setting the temperature to 85 ℃ after the addition is finished, reducing the stirring frequency to 30HZ, slowly heating, controlling the heating time to 20min, setting the temperature to 85 ℃, keeping the temperature for 30min, and stirring at a constant speed;
c. adding the balance of pure water to 1000L, and performing auxiliary cooling to a set value of 40 ℃;
(2) warping slashing
The operating speed of the warping slasher is 180 m/min; the crimp tension was 20N; the grouting pressure is 0.5 Mpa; the temperature of the slurry tank is 40 ℃; the oven temperature is 130 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving the grey cloth is 700rpm, and the let-off tension is 350N; TW angle 240 °; the main spraying pressure is 3.5 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 30 m/min; the rotating speed of the roller is 500 rpm; the temperature of the hot water tank is 40 ℃; the drying temperature is 65 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 270 540
2 270 270 780
3 270 390 360
4 390 390 1080
(6) FN surface treatment
The running speed of the FN surface treatment machine is 80 m/min; the sending tension is 160N; the crimp tension was 220N; the drying temperature is 125 ℃.
Comparative example 3
An opening process of electronic-grade glass fiber cloth, which uses the specification of 1080 of the electronic-grade glass fiber cloth, comprises the following steps:
(1) preparation of slurry
a. Adding 500L of pure water into a clean liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43 HZ;
b. slowly adding 5.0% PVA5-88 by mass ratio for 3min, circulating for about 2min, setting the temperature to 85 deg.C after adding, reducing stirring frequency to 30HZ, slowly heating for 20min, setting the temperature at 85 deg.C, keeping the temperature for 30min, and stirring at uniform speed;
c. adding pure water for auxiliary cooling, and cooling to a set value of 40 ℃;
d. adding 0.1 percent of fatty alcohol-polyoxyethylene ether, 0.1 percent of methanol and the balance of pure water by mass percent to 1000L, and continuously stirring for later use.
(2) Warping slashing
The operating speed of the warping slasher is 180 m/min; the crimp tension was 20N; the grouting pressure is 0.5 Mpa; the temperature of the pulp tank is 40 ℃; the oven temperature is 130 ℃;
(3) woven grey cloth
The running speed of a weaving machine for weaving the grey cloth is 700rpm, and the let-off tension is 350N; the TW angle is 240 °; the main spraying pressure is 3.5 kgf;
(4) splitting grey cloth
The running speed of a grey cloth splitting machine is 30 m/min; the rotating speed of the roller is 500 rpm; the temperature of the hot water tank is 40 ℃; the drying temperature is 65 ℃;
(5) BH smoldering
The BH smoldering stage is divided into four temperature rising stages, and the temperature rising curve is shown in a table 1;
TABLE 1 temperature-rising curve data table for BH smoldering process
Phases Onset temperature/. degree.C End temperature/. degree.C Time/min
1 At room temperature 270 540
2 270 270 780
3 270 390 360
4 390 390 1380
(6) FN surface treatment
The running speed of the FN surface treatment machine is 80 m/min; the sending tension is 160N; the crimp tension was 220N; the drying temperature was 125 ℃.
Combustible materials before and after the treatment of the grey cloth, tension and impregnation time of the grey cloth after the treatment in the splitting process of the examples 1-3 and the comparative examples 1-3 are detected according to IPC-4412 standard, and three groups of parallel samples are made for each, wherein: the reduction ratio of the greige cloth opening combustible material is (greige cloth combustible material-greige cloth opening combustible material) multiplied by 100 per greige cloth combustible material;
BH combustible reduction ratio/% (grey cloth combustible-BH combustible) x 100/grey cloth combustible;
the results of tests of examples 1 to 3 are shown in Table 2, and the results of tests of comparative examples 1 to 3 are shown in Table 3;
table 2 results of tests in examples 1 to 3
Figure BDA0003553742230000101
TABLE 3 test results of comparative examples 1 to 3
Figure BDA0003553742230000102
Figure BDA0003553742230000111
As can be seen from tables 2 and 3, compared with the conventional size, under the same condition of the grey cloth splitting process, the size can be removed by about 83%, the conventional size can be removed by only about 63%, the size removal ratio is improved by about 20%, the impregnation performance shows that the size can be used for producing the glass cloth 22S, the conventional size can be used for producing the glass cloth 39S, the ratio is reduced by 40%, and the invention is more beneficial to the permeation of the glass cloth and resin; by using the slurry disclosed by the invention and the traditional slurry, the traditional slurry can reach the slurry removal proportion of about 99% under the BH smoldering condition of 51 hours, but the slurry disclosed by the invention can reach the slurry removal proportion under the BH smoldering condition of 46 hours, the performance is excellent in the aspect of reducing the strength loss, the strength of the glass cloth produced by using the slurry disclosed by the invention is improved by about 30%, and the performance of the glass cloth is ensured.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.

Claims (10)

1. The fiber opening process easy to clean the electronic-grade glass fiber cloth slurry is characterized by comprising the following steps of: size preparation → warping slashing → weaving gray fabric → fiber opening of gray fabric → BH braising → FN surface treatment.
2. The opening process easy to clean by the slurry of the electronic-grade glass fiber cloth according to claim 1, characterized in that the slurry preparation step comprises:
(1) adding pure water into the liquid preparation cylinder, starting a stirrer, and setting the frequency to be 43-50 HZ;
(2) adding polyvinyl alcohol for 3-10min, circulating for 2-3min, reducing stirring frequency to 30-35HZ, heating to 85-95 deg.C, maintaining for 20-25min, and maintaining for 30-40 min;
(3) cooling to 40-50 ℃, adding the auxiliary agent A, the auxiliary agent B and the balance of pure water, and continuing stirring for later use.
3. The fiber opening process easy to clean the electronic grade glass fiber cloth slurry according to claim 1, characterized in that the operating speed of a warping slasher is 60-180 m/min; the curling tension is 10-20N; the grouting pressure is 0.4-0.5 Mpa; the temperature of the pulp tank is 40-50 ℃; the oven temperature was 100-130 ℃.
4. The opening process easy to clean the sizing agent of the electronic-grade glass fiber cloth as claimed in claim 1, wherein the running speed of a weaving machine for weaving the grey cloth is 500-700rpm, and the let-off tension is 80-350N; the TW angle was 225-240 °; the main spraying pressure is 1.0-3.5 kgf.
5. The opening process easy to clean the sizing agent of the electronic-grade glass fiber cloth according to claim 1, characterized in that the running speed of a machine in the opening of the grey cloth is 15-30 m/min; the rotating speed of the roller is 200-500 rpm; the temperature of the hot water tank is 40-50 ℃; the drying temperature is 55-65 ℃.
6. The opening process easy to clean for the slurry of the electronic grade glass fiber cloth according to claim 1, characterized in that the BH smoldering stage is divided into four temperature raising stages: the first stage is that the room temperature is increased to 260-270 ℃ for 400-540 min; the second stage is a maintaining stage, wherein the temperature is maintained at 260-270 ℃ and the time is 660-780 min; the third stage is that the temperature is increased from 260 ℃ to 380 ℃ and 390 ℃ for 240 ℃ and 360 min; the second stage is a maintaining stage, wherein the temperature is maintained at 380-.
7. The opening process easy to clean of the electronic grade glass fiber cloth slurry as claimed in claim 1, wherein the running speed of the FN surface treatment machine is 50-80 m/min; the sending tension is 100-160N; the curling tension is 120-220N; the drying temperature is 105-125 ℃.
8. The sizing agent easy to clean for the sizing agent of the electronic-grade glass fiber cloth of any one of claims 1 to 7 is characterized by being prepared from the following raw materials in percentage by mass:
Figure FDA0003553742220000011
Figure FDA0003553742220000021
9. the paste easy to clean of electronic grade fiberglass cloth paste of claim 8, wherein: the alcoholysis degree dB of the polyvinyl alcohol is 78-82%, and the polymerization degree n is 300-400.
10. The paste easy to clean of electronic grade glass fiber cloth paste according to claim 8, characterized in that: the auxiliary agent A is fatty alcohol-polyoxyethylene ether; the auxiliary agent B is micromolecular alcohol.
CN202210278895.XA 2022-03-18 2022-03-18 Splitting process easy to clean electronic-grade glass fiber cloth slurry and slurry used in splitting process Pending CN114645365A (en)

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