CN1321239C - Post-treatment process for electronic-grade fiberglass cloth - Google Patents

Post-treatment process for electronic-grade fiberglass cloth Download PDF

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Publication number
CN1321239C
CN1321239C CNB2005100215112A CN200510021511A CN1321239C CN 1321239 C CN1321239 C CN 1321239C CN B2005100215112 A CNB2005100215112 A CN B2005100215112A CN 200510021511 A CN200510021511 A CN 200510021511A CN 1321239 C CN1321239 C CN 1321239C
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destarch
stove
fiberglass cloth
baking temperature
cloth
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CN1730771A (en
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郭炯
赵棣
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Sichuan Tianquan Electronic Materials Co.,Ltd.
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SICHUAN GLASS FIBER CO Ltd
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Abstract

The present invention discloses a post-treatment technology for an electronic-grade fiberglass cloth. An undesized fiberglass cloth which is obtained after the weaving of a rapier loom is directly desized through a thermal desizing furnace, and a fiberglass cloth, the whiteness of which is more than 70, is obtained, and the residual quantity of organic matter of the fiberglass cloth is below 0.05%; coupling agent impregnation is carried out via a vertical machine set to obtain a finished product. The technology of the present invention is adopted. The existing pre-desizing working procedure is decreased in the present invention. The investment of post-treatment equipment and the labour cost are greatly saved. The manufacturing cost is reduced, and the product quality of the electron-grade fiberglass cloth can be increased.

Description

Post-treatment process for electronic-grade fiberglass cloth
Technical field
The present invention relates to a kind of glass fabric and weave cotton cloth the back, relate generally to post-treatment process for electronic-grade fiberglass cloth the destarch treatment process of cloth.
Technical background
In the prior art, what electronic-grade glass fiber cloth was widely used in that electron trade produces different-thickness covers copper sheet (PCB), and in the production of electronic-grade glass fiber cloth, because the restriction of factors such as raw material when making glass fibre early stage and manufacturing technique, glass cloth is to use the air-jet loom weaving moulding, air-jet loom be starch type G75 tank furnace yarn with yarn, the loom rotating speed is 700-800r/min, the yarn mode of drawing that adopts major-minor nozzle to combine with special-shaped reed, and starch type G75 tank furnace yarn weave cotton cloth the back just must be through the pre-destarch operation of vertical unit, all be to adopt the pre-destarch of the vertical unit-hot destarch of processing stove-vertical unit coupling agent dipping-check to the aftertreatment technology of glass fabric therefore in the later stage, the treatment process of packing.In previous process steps, the main purpose of the pre-destarch of vertical unit is that the organic substance residues amount on the cloth is reduced to 0.5%, and reduce its loss of strength as far as possible, handling the hot destarch of stove is to be combustion medium with the natural gas, the cloth that the body of heater of employing hot air circulation mode is handled pre-destarch carries out degreasing (removing the organic substance residues amount) again, its residual quantity is reduced to below 0.05%, the whiteness of cloth is greater than 70, and vertical unit coupling agent dipping mainly is the cloth after the destarch to be carried out proceeding oven dry after the silane coupler aqueous solution floods batch.Like this, not only the aftertreatment technology complexity, the control step is many and be difficult for accurately control, the processing time is long, and the post processing equipment costliness, operates manually also a lot, has increased the production cost of glass fabric greatly.
Summary of the invention
The objective of the invention is to overcome above-mentioned technological deficiency, a kind of post-treatment process for electronic-grade fiberglass cloth is provided.Adopt technology of the present invention, will be through the weave cotton cloth glass fabric of the not destarch that obtains of loom, directly carry out hot destarch by hot destarch stove, reduced original pre-destarch operation, save post processing equipment investment and labour cost greatly, reduce production costs, and can improve the product quality of electronic-grade glass fiber cloth.
The present invention is achieved through the following technical solutions:
Post-treatment process for electronic-grade fiberglass cloth, it is characterized in that: the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.
Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.
The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 400-560 ℃, and stoving time is 25-37 hour; The baking temperature in middle level is set to 400-560 ℃, and stoving time is 25-37 hour; The baking temperature of lower floor is set to 400-560 ℃, and stoving time is 25-37 hour.
Described vertical unit is meant vertical dipping unit, i.e. up earlier the after fabric guide roll of glass cloth dipping back oven dry running route in descending operation, batch.
Described loom is arrow shaft or air-jet loom.
Described destarch is meant: remove the sizing agent on the glass cloth.
The organic substance residues amount is to be meant below 0.05% after hot destarch that the content of organics on the cloth is compared before the content of organics on the glass fabric and hot destarch to drop to below 0.05%.
Described coupling agent dipping is meant that glass fabric is proceeded oven dry behind silane coupler aqueous solution dipping batch.
Described finished product be meant on the glass fabric combustible content more than 0.18%, whiteness is that 300N/ (25 * 100) mm broadwise is that 230N/ (25 * 100) mm, weight are 203.4 ± 15 gram/rice greater than 70, through the fracture strength warp-wise of broadwise 2, thread count is 17.4 ± 1 pieces/centimetre of warp-wises, broadwise is that 12.2 ± 1 pieces/centimetre, thickness are 0.2 ± 0.02mm.
In the present invention, owing in the production process of glass fibre in early stage, the glass fiber infiltration agent that uses has been carried out prescription adjustment, the chemical composition of sizing agent finished product is made up of paraffin, machine oil, oleic acid, fatty alcohol-polyoxyethylene ether, dibutyl phthalate, hexadecyl trimethyl ammonium bromide, color-fixing agent G, and the weight portion of its component is: paraffin 1-3 part; Machine oil 1-2.5 part; Oleic acid 0.5-2 part; Fatty alcohol-polyoxyethylene ether 0.5-1.2 part; Dibutyl phthalate 0.1-1.5 part; Hexadecyl trimethyl ammonium bromide 0.1-1 part; Color-fixing agent G2.5-5 part.Because its chemical property of the synthetic back of each raw material of sizing agent determines, is mainly color-fixing agent G and can not decomposes in pre-destarch process, therefore just can reduce pre-destarch operation, and directly carry out hot destarch.
The invention has the advantages that:
1, owing to adopts Rapier looms to weave cotton cloth, and Rapier looms can use paraffin wax type and starch type tank furnace yarn with yarn, all can weave EW200-127 cloth by the longitude and latitude combination, it is electronic-grade glass fiber cloth, its rotating speed is 180-200r/min, filling insertion way is a sword head wefting insertion, and Rapier looms is lower than the price of air-jet loom comparatively speaking, has so just saved equipment investment cost greatly.
2, being used for the processing stove that hot destarch baking handles is to be single seat structure electric furnace, be divided into., in., lower floor control, be every layer and be closed-loop control system, adopt three-phase controllable silicon pressure regulation (merit) device respectively, sensor adopts K type thermocouple, temperature controller adopts SR93 type (AT function, the PID computing is regulated) to form closed-loop system and controls, by instrument scale parameter 0-20 being set, being the output of instrument and the adjusting rule that input keeps certain relation: Δ I=-K Δ X.Wherein K is a scale parameter.Integral parameter 00-60min, differential parameter 0-60min make the temperature controlling accuracy reach ± 0 ℃-± 10 ℃, and pass through the baking temperature of processing stove and the control of time, make that the organic matter thing is reduced to below 0.05 on the cloth, the whiteness of cloth has improved the product quality of glass fabric greater than 70.
3, reduced pre-destarch operation in the science and engineering skill of original place, directly cloth has been carried out hot destarch, saved like this, greatly reduced production cost nearly ten million yuan of the equipment investment of pre-destarch operation.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
Embodiment 1
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 400 ℃, and stoving time is 25 hours; The baking temperature in middle level is set to 400 ℃, and stoving time is 25 hours; The baking temperature of lower floor is set to 400 ℃, and stoving time is 25 hours.
Embodiment 2
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 560 ℃, and stoving time is 37 hours; The baking temperature in middle level is set to 560 ℃, and stoving time is 37 hours; The baking temperature of lower floor is set to 560 ℃, and stoving time is 37 hours.
Embodiment 3
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 460 ℃, and stoving time is 27 hours; The baking temperature in middle level is set to 460 ℃, and stoving time is 27 hours; The baking temperature of lower floor is set to 460 ℃, and stoving time is 27 hours.
Embodiment 4
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 480 ℃, and stoving time is 29 hours; The baking temperature in middle level is set to 480 ℃, and stoving time is 29 hours; The baking temperature of lower floor is set to 480 ℃, and stoving time is 29 hours.
Embodiment 5
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 500 ℃, and stoving time is 30 hours; The baking temperature in middle level is set to 500 ℃, and stoving time is 30 hours; The baking temperature of lower floor is set to 500 ℃, and stoving time is 30 hours.
Embodiment 6
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 525 ℃, and stoving time is 35 hours; The baking temperature in middle level is set to 525 ℃, and stoving time is 35 hours; The baking temperature of lower floor is set to 525 ℃, and stoving time is 35 hours.
Embodiment 7
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 545 ℃, and stoving time is 36 hours; The baking temperature in middle level is set to 545 ℃, and stoving time is 36 hours; The baking temperature of lower floor is set to 525 ℃, and stoving time is 36 hours.
Embodiment 8
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 550 ℃, and stoving time is 36 hours; The baking temperature in middle level is set to 550 ℃, and stoving time is 36 hours; The baking temperature of lower floor is set to 550 ℃, and stoving time is 36 hours.
Embodiment 9
Post-treatment process for electronic-grade fiberglass cloth, the glass fabric of the not destarch that after loom is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product.Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively.The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 558 ℃, and stoving time is 36.5 hours; The baking temperature in middle level is set to 558 ℃, and stoving time is 36.5 hours; The baking temperature of lower floor is set to 558 ℃, and stoving time is 36.5 hours.
In the present invention, to in the production process of glass fibre in early stage the glass fiber infiltration agent that uses having been carried out prescription adjustment, the chemical composition of sizing agent finished product is made up of paraffin, machine oil, oleic acid, fatty alcohol-polyoxyethylene ether, dibutyl phthalate, hexadecyl trimethyl ammonium bromide, color-fixing agent G, and the weight portion of its component is: paraffin 1-3 part; Machine oil 1-2.5 part; Oleic acid 0.5-2 part; Fatty alcohol-polyoxyethylene ether 0.5-1.2 part; Dibutyl phthalate 0.1-1.5 part; Hexadecyl trimethyl ammonium bromide 0.1-1 part; Color-fixing agent G2.5-5 part.
The preparation method of above-mentioned glass fiber infiltration agent is:
A, take by weighing machine oil 1-2.5 part, paraffin 1-3 part, oleic acid 0.5-2 part, dibutyl phthalate 0.1-1.5 part, fatty alcohol-polyoxyethylene ether 0.5-1.2 part respectively according to the weight portion of prescription and put into reactor, and unlatching steam, the steam pressure list index must not surpass 2 * 0.1mpa, when temperature of reaction kettle starts agitator after 7~10 minutes during at 60~65 ℃ or after opening steam, stir on one side, continue heating on one side, mixing speed is 50-100 rev/min;
B, when reactor temperature reaches 70~80 ℃, steam off, oil temperature rises to 85~90 ℃ naturally, waits for 15~20 minutes, adds temperature again and be 45~50 ℃ color-fixing agent G2.5-5, when adding color-fixing agent G, oily temperature must not be lower than 84-86 ℃;
C, add hot water more than 90 ℃ again after adding color-fixing agent G10 minute, promptly add 0.2-0.4 kilogram hot water more than 90 ℃ for the first time by per 100 kilograms of sizing agents, added one time hot water 0.2-0.4 kilogram later on every 5 minutes, when the oil phase retrogradation is close, stirred 5 minutes earlier, add 0.2-0.4 kilogram hot water more than 90 ℃ again, added the kilogram of hot water 0.2-0.4 more than 90 ℃ later on every 3 minutes one time, mixing speed is 50-100 rev/min;
D, when oil phase changes thin or faint yellow, added 1~1.5 kilogram 50-90 ℃ hot water in then per 3 minutes, after 10 minutes, at the hot water of 70~75 ℃ of second paddle place addings of reactor, this moment, oily temperature must not be lower than 70-75 ℃, stirred 5 minutes, mixing speed is 50-100 rev/min, add soft water, make its liquid surface, continue stirring and beat to blending tank standby after 2 minutes apart from reactor upper port 2-3 centimeters;
E, dilution hexadecyl trimethyl ammonium bromide: is 1: 20 dilution proportion hexadecyl trimethyl ammonium bromide by hexadecyl trimethyl ammonium bromide than 50-80 ℃ of hot water, stirs and beats after 2 minutes to blending tank and above-mentioned d step gained liquid mixing;
F, with after the removal of impurity of above-mentioned e step gained liquid filtering, add soft water dilution again, soft water and dense oily dilution ratio 1: 2-5, it is standby to obtain the sizing agent finished product.
In the above-mentioned b-d step, add the water time to be not less than 40 minutes.

Claims (1)

1, post-treatment process for electronic-grade fiberglass cloth, it is characterized in that: the glass fabric of the not destarch that after Rapier looms is weaved cotton cloth, obtains, directly carry out hot destarch by hot destarch stove, to obtain the organic substance residues amount be below 0.05% and whiteness greater than 70 glass fabric, carry out the coupling agent dipping by vertical unit again, obtain finished product; Described hot destarch stove is a single seat structure electric furnace, is divided into upper, middle and lower layer control, and every layer is closed-loop control system, adopts the three-phase controllable silicon regulator, sensor, the temperature controller that are electrically connected to form closed-loop system respectively; The baking temperature on described hot destarch stove its upper strata when hot destarch is set to 400-560 ℃, and stoving time is 25-37 hour; The baking temperature in middle level is set to 400-560 ℃, and stoving time is 25-37 hour; The baking temperature of lower floor is set to 400-560 ℃, and stoving time is 25-37 hour.
CNB2005100215112A 2005-08-23 2005-08-23 Post-treatment process for electronic-grade fiberglass cloth Active CN1321239C (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101532229B (en) * 2009-03-12 2011-12-07 珠海富华复合材料有限公司 Process for flattening post treatment of electronic grade glass fiber cloth
CN101871149B (en) * 2010-06-04 2011-09-07 上海宏和电子材料有限公司 Fiber opening method for electronic grade glass fiber cloth and electronic grade glass fiber cloth obtained by using same
CN102926183A (en) * 2012-10-31 2013-02-13 上海宏和电子材料有限公司 Application of assistant agent in electronic-grade glass fiber cloth desizing and desizing process thereof
JP2022021666A (en) * 2020-07-22 2022-02-03 旭化成株式会社 Glass cloth, prepreg and printed wiring board
CN115418815B (en) * 2022-08-15 2023-05-16 四川省玻纤集团有限公司 Surface treatment method and surface treatment system for electronic grade glass fiber cloth

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Publication number Priority date Publication date Assignee Title
JPH03167357A (en) * 1989-11-28 1991-07-19 Shin Kobe Electric Mach Co Ltd Production of glass non-woven fabric for laminate and production of laminate
US5584965A (en) * 1992-07-07 1996-12-17 Shin-Kobe Electric Machinery Co., Ltd. Method of producing a laminate of glass fiber non-woven fabric base material
JP3167357B2 (en) * 1991-07-15 2001-05-21 タジマサービス株式会社 Double floor structure
CN1546408A (en) * 2003-12-11 2004-11-17 峻 章 Water dispersable glass fiber sizing material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03167357A (en) * 1989-11-28 1991-07-19 Shin Kobe Electric Mach Co Ltd Production of glass non-woven fabric for laminate and production of laminate
JP3167357B2 (en) * 1991-07-15 2001-05-21 タジマサービス株式会社 Double floor structure
US5584965A (en) * 1992-07-07 1996-12-17 Shin-Kobe Electric Machinery Co., Ltd. Method of producing a laminate of glass fiber non-woven fabric base material
CN1546408A (en) * 2003-12-11 2004-11-17 峻 章 Water dispersable glass fiber sizing material

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