CN111977990A - High-performance impregnating compound for superfine electronic yarn and preparation method thereof - Google Patents

High-performance impregnating compound for superfine electronic yarn and preparation method thereof Download PDF

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CN111977990A
CN111977990A CN202010934415.1A CN202010934415A CN111977990A CN 111977990 A CN111977990 A CN 111977990A CN 202010934415 A CN202010934415 A CN 202010934415A CN 111977990 A CN111977990 A CN 111977990A
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starch
parts
electronic
impregnating compound
superfine
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CN111977990B (en
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张国平
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Qingyuan Zhongxin Century Electronic Material Co., Ltd
Qingyuan Zhongxin Electronic Materials Co.,Ltd.
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Qingyuan Zhongxin Shiji Glass Fiber Co ltd
Qingyuan Zhongxin Electronic Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/465Coatings containing composite materials
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/26Macromolecular compounds or prepolymers
    • C03C25/32Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C03C25/321Starch; Starch derivatives
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/40Organo-silicon compounds

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  • Geochemistry & Mineralogy (AREA)
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  • Composite Materials (AREA)
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Abstract

The invention discloses an ultrafine electronic yarn impregnating compound and a preparation method thereof, wherein the impregnating compound comprises an active component of the ultrafine electronic yarn impregnating compound with the mass fraction of 6.5-7% and the balance of water; the active component comprises the following raw materials in parts by weight: 44-65.7 parts of starch, 9-15 parts of mixed grease, 0.8-2.2 parts of aliphatic polyamide, 2.6-5.1 parts of fatty acid ester lubricant, 0.7-2.1 parts of nonionic active agent, 5.2-9.6 parts of hydrogenated vegetable oil, 2.8-5.1 parts of cationic lubricant, 6.8-12.2 parts of coupling agent, 0.7-2.3 parts of preservative and 0.01-0.04 part of defoaming agent; the starch consists of the starch HR and the starch HJ, the invention solves the quality problem of the traditional sizing agent applied to the superfine electronic yarn, has excellent antiseptic effect, can be maintained for more than 24 hours, and eliminates the harm of formaldehyde volatilization to human bodies.

Description

High-performance impregnating compound for superfine electronic yarn and preparation method thereof
Technical Field
The invention relates to the field of industrial production of glass fibers, in particular to a high-performance impregnating compound for superfine electronic yarns and a preparation method thereof.
Background
The glass fiber electronic yarn is formed by twisting continuous glass strands, electronic cloth is formed by weaving, and the glass fiber electronic yarn is made into a Copper-Clad plate (Copper Clad Laminate) and then is used for electronic industrial products such as Printed Circuit boards (Printed Circuit boards) and the like. The raw materials for the copper-clad plate substrate mainly comprise a glass fiber cloth base, a paper base, a metal base and the like. The copper-clad plate is a basic material of a printed circuit board, and the printed circuit board is an important carrier of electronic communication equipment. The glass fiber electronic yarn is different from other industrial glass fiber spun yarns and is thinner than other glass fiber yarns, the diameter range of a single fiber is generally 3.5-9 mu m, and the fineness range of the glass fiber electronic yarn is 3.3-136 tex.
In recent years, electronic information communication technology has further developed with the development of industrial internet, new energy automobiles and the like, and thus, the demand for glass fiber electronic yarn and electronic cloth has been continuously increased. In order to achieve the purpose of higher speed and more reliable information transmission, the requirements on the printed circuit board and the copper-clad plate are higher, and the requirements on the glass fiber electronic cloth and the electronic yarn are also more rigorous. Currently, in order to meet the requirements of high-grade printed circuit boards, the thickness of electronic cloth needs to reach 0.03mm or less.
Although China is always in the largest glass fiber export state in the world, deep processing of the glass fiber electronic yarn industry is still urgent, and advanced product research and development and the highest manufacturing technology are mainly concentrated in countries such as Europe, America and Japan. The electronic cloth is divided into thick (more than 0.151mm), thin (0.15-0.051mm), ultra-thin (0.05-0.026mm) and ultra-thin (less than 0.025mm) according to the thickness. According to the standard, the higher level of the electronic cloth produced in China at present is 1067 cloth, the thickness of the electronic cloth is about 0.032mm, and the corresponding yarn fineness is 5.6 tex; and the electronic cloth woven abroad, especially Japan, reaches dozens of microns, such as 1037 (thickness 0.025mm), 1027 (thickness 0.020mm) and 1017 (thickness 0.015mm) cloth manufactured by Nidong textile company, and the fineness of the used glass fiber electronic yarn is as fine as 4.3tex, 3.3tex and 1.7 tex. Therefore, the superfine development of the glass fiber electronic yarn is a problem to be solved and overcome urgently in China.
The impregnating compound is an indispensable material in the drawing and weaving of the glass fiber, plays the roles of bonding, bundling, lubricating and wear-resisting the fiber, eliminating static electricity and the like, can effectively lubricate the surface of the glass fiber, can integrate hundreds of and even thousands of glass fiber monofilaments into a bundle, can change the surface state of the glass fiber, and meets the requirements of the subsequent process processability of the glass fiber precursor.
The impregnating compound with the traditional formula is only suitable for the production of E glass fibers with the conventional diameter, has a plurality of defects influencing the product quality when being applied to the production of glass fibers with the superfine diameter, and is not suitable for the production application of superfine yarns, such as: (1) the phenomenon of inner and outer layer migration is serious; (2) static electricity cannot be eliminated, so that subsequent processing is influenced; (3) the powder is seriously removed in the process of adding; (4) the glass fiber is easy to break during drawing and forming, so that the operation is unstable; (5) the hairiness rate is high.
CN101575177A discloses an impregnating compound for reducing the hairiness of superfine electronic yarns, which comprises starch, a cationic lubricant, a central lubricant, an emulsifier, polyethylene oxide, a silicon coupling agent, an auxiliary film-forming agent, a preservative, an antistatic agent and water, wherein the impregnating compound prepared by the invention has an obvious effect of reducing the hairiness of superfine glass fibers, the hairiness of the drawn D450 superfine glass fiber yarns is 9-21/500 m, and the monofilament strength is 0.59-0.65N/Tex. However, the original formula uses formaldehyde as a preservative, and the formaldehyde can volatilize in the operation process, so that the health of a human body is influenced, the preservative time is short, and the preservative can only be maintained for about 10 hours; meanwhile, the broken rate of the glass fiber is high during wire drawing forming, the rate of finished products is influenced, and the production cost is high.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-performance impregnating compound for superfine electronic yarns and a preparation method thereof, which solve the quality problem of the traditional impregnating compound applied to the superfine electronic yarns, and simultaneously use a preservative FS14D to replace formaldehyde, so that the high-performance impregnating compound is excellent in corrosion prevention effect, can be maintained for more than 24 hours, and simultaneously eliminates the harm of formaldehyde volatilization to human bodies.
In order to achieve the purpose, the invention adopts the following technical scheme:
an ultrafine electronic yarn impregnating compound comprises an active component of the ultrafine electronic yarn impregnating compound with the mass fraction of 6.5-7% and the balance of water;
the superfine electronic yarn impregnating compound comprises the following active components in parts by weight: 44-65.7 parts of starch, 9-15 parts of mixed grease, 0.8-2.2 parts of aliphatic polyamide, 2.6-5.1 parts of fatty acid ester lubricant, 0.7-2.1 parts of nonionic active agent, 5.2-9.6 parts of hydrogenated vegetable oil, 2.8-5.1 parts of cationic lubricant, 6.8-12.2 parts of coupling agent, 0.7-2.3 parts of preservative and 0.01-0.04 part of defoaming agent;
the starch consists of starch HR and starch HJ.
Preferably, the weight ratio of the starch HR to the starch HJ in the starch is 31-43: 15-21.
Preferably, the weight ratio of the starch HR to the starch HJ in the starch is 38.2-51.2: 8.8-14.5.
Preferably, the weight ratio of the starch HR to the starch HJ in the starch is 22-31: 22-31.
Preferably, the mixed grease is mixed grease AM.
Preferably, the cationic lubricant is a cationic lubricant E-SO.
Preferably, the preservative is FS-14D.
Preferably, the coupling agent is a silane coupling agent.
The invention also provides a preparation method of the superfine electronic yarn impregnating compound, which comprises the following steps:
(1) mixing the starch with the formula amount and water, stirring, heating, preserving heat and cooling to obtain a gelatinized starch solution;
(2) mixing the mixed grease, the aliphatic polyamide, the fatty acid ester lubricant, the nonionic active agent, the hydrogenated vegetable oil, the cationic lubricant, the coupling agent, the preservative and the defoaming agent according to the formula ratio, and uniformly stirring to obtain the aid;
(3) mixing the auxiliary agent obtained in the step (2) with the gelatinized starch solution obtained in the step (1) for reaction, and forming an emulsion after the temperature is stable to obtain the superfine electronic yarn impregnating compound;
in the step (1), the heating and heat preservation is carried out at 96 ℃ for 30 min; the temperature is reduced to 76 ℃;
the temperature after the temperature stabilization in the step (3) is 60 ℃.
The invention also provides the application of the superfine electronic yarn impregnating compound in the production of superfine glass fiber electronic yarns.
The invention has the beneficial effects that:
(1) the novel starch HR and the novel starch HJ are used, and the novel starch HR and the novel starch HJ are screened and compounded to form a novel molecular structure, improve the reaction combination mode of molecules of the impregnating compound and superfine yarns, and change the effective combination degree of other auxiliary agents between the starch and the surfaces of glass fibers, so that the combination between the impregnating compound and the surfaces of the superfine yarn glass fibers is firmer, and the physical and chemical properties of the combined finished product are better.
(2) The superfine electronic yarn is difficult to accept sizing agents with large viscosity fluctuation, the pH value of the superfine electronic yarn high-performance sizing agent emulsion is 5.32-5.6, the viscosity value is 8.0-8.4cps, the stability is better, and the superfine electronic yarn is more suitable for producing superfine yarn glass fiber electronic yarns.
(3) The superfine electronic yarn impregnating compound disclosed by the invention adopts the preservative FS14D to eliminate the harm of formaldehyde volatilization to a human body, so that the preservative aging is prolonged, and meanwhile, the superfine electronic yarn impregnating compound can participate in the reaction of other components of the impregnating compound, the bundling effect of the impregnating compound is optimized, and the film forming strength of the impregnating compound is improved; the prepared sizing agent can be used for producing superfine electronic yarns with the monofilament diameter of 3.81-4 microns, the phenomenon of migration of the inner layer and the outer layer can be effectively avoided, the breakage rate of the prepared glass fiber is reduced, the hairiness rate is obviously reduced, the product quality is greatly improved, and the product rate is over 90 percent.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In the present invention, the source of the raw material used is not limited, and unless otherwise specified, the raw material used in the present invention is a commercially available product of ordinary skill in the art, wherein the aliphatic polyamide is available from Gimura oil chemical Co., Ltd., product number ZY-51; a fatty acid ester lubricant, available from TAIAN Shadan Sheng daily applied materials, Inc., having a LUB-1 designation; the nonionic active agent is purchased from bamboo oil and fat Co, and has the product number of GF-1; hydrogenated vegetable oil was purchased from adico, under the AM brand name; the cationic lubricant is purchased from advanced chemical technology, Inc., and has the product number of ESO; the coupling agent was purchased from Toho chemical industry Co., Ltd, with a product number of GF-08; the preservative was purchased from Daihu chemical industries, Inc. under the trade designation FS-14D; the antifoaming agent is purchased from Gnaphalium chinensis Sims Gnaphalium, four New science and technology application research institute, and has a product number of S-29; the starch HR is purchased from Jurashiki Kaisha of Japan chemical, and has a product number of HR; starch HJ was purchased from Jurashiki Kaisha of Japan chemical, and its product number is HJ.
Basic embodiment
An ultrafine electronic yarn impregnating compound comprises an active component of the ultrafine electronic yarn impregnating compound with the mass fraction of 6.5-7% and the balance of water;
the superfine electronic yarn impregnating compound comprises the following active components in parts by weight: 44-65.7 parts of starch, 9-15 parts of mixed grease, 0.8-2.2 parts of aliphatic polyamide, 2.6-5.1 parts of fatty acid ester lubricant, 0.7-2.1 parts of nonionic active agent, 5.2-9.6 parts of hydrogenated vegetable oil, 2.8-5.1 parts of cationic lubricant, 6.8-12.2 parts of coupling agent, 0.7-2.3 parts of preservative and 0.01-0.04 part of defoaming agent;
the starch consists of starch HR and starch HJ.
Preferably, the weight ratio of the starch HR to the starch HJ in the starch is 31-43: 15-21.
Preferably, the weight ratio of the starch HR to the starch HJ in the starch is 38.2-51.2: 8.8-14.5.
Preferably, the weight ratio of the starch HR to the starch HJ in the starch is 22-31: 22-31.
Preferably, the mixed grease is mixed grease AM.
Preferably, the cationic lubricant is a cationic lubricant E-SO.
Preferably, the preservative is FS-14D.
Preferably, the coupling agent is a silane coupling agent.
The invention also provides a preparation method of the superfine electronic yarn impregnating compound, which comprises the following steps:
(1) mixing the starch with the formula amount and water, stirring, heating, preserving heat and cooling to obtain a gelatinized starch solution;
(2) mixing the mixed grease, the aliphatic polyamide, the fatty acid ester lubricant, the nonionic active agent, the hydrogenated vegetable oil, the cationic lubricant, the coupling agent, the preservative and the defoaming agent according to the formula ratio, and uniformly stirring to obtain the aid;
(3) mixing the auxiliary agent obtained in the step (2) with the gelatinized starch solution obtained in the step (1) for reaction, and forming an emulsion after the temperature is stable to obtain the superfine electronic yarn impregnating compound;
in the step (1), the heating and heat preservation is carried out at 96 ℃ for 30 min; the temperature is reduced to 76 ℃;
the temperature after the temperature stabilization in the step (3) is 60 ℃.
The invention also provides the application of the superfine electronic yarn impregnating compound in the production of superfine glass fiber electronic yarns.
Example 1-4 an ultra-fine electronic yarn treating compound and a method for preparing the same
The compositions and amounts of the ultra-fine electronic yarn size described in examples 1-4 are shown in Table 1.
TABLE 1
Figure BDA0002671420550000051
Figure BDA0002671420550000061
The preparation method of the superfine electronic yarn impregnating compound comprises the following steps:
(1) mixing the starch with the formula amount and water, stirring, heating at 96 ℃ and keeping the temperature for 30min, and cooling to 76 ℃ to obtain a gelatinized starch solution;
(2) mixing the mixed grease, the aliphatic polyamide, the fatty acid ester lubricant, the nonionic active agent, the hydrogenated vegetable oil, the cationic lubricant, the coupling agent, the preservative and the defoaming agent according to the formula ratio, and uniformly stirring to obtain the aid;
(3) and (3) mixing the auxiliary agent obtained in the step (2) with the gelatinized starch solution obtained in the step (1) for reaction, and forming emulsion after the temperature is stabilized at 60 ℃ to obtain the superfine electronic yarn impregnating compound.
Comparative example 1 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 4 in that the starch is only starch HR.
Comparative example 2 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 4 in that the starch is only starch HJ.
Comparative example 3 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 4 in that the starch HR is replaced by an unmodified hybrid corn starch with a linear chain of 70%; starch HJ was replaced by an etherified hybrid maize starch with 27% amylose.
Comparative example 4 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 4 in that the weight ratio of starch HR and starch HJ was 30: 25.
Comparative example 5 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 4 in that an epoxy derivative of 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexylformate epoxy resin and 1, 2-epoxy-3- (di-2, 6-xylylmethoxy) propane in a mass ratio of 6:1 was used in place of the coupling agent.
Comparative example 6 superfine electronic yarn impregnating compound and preparation method thereof
The difference between the comparative example and example 4 is that the active component comprises 16 parts of mixed grease, 2.4 parts of aliphatic polyamide, 0.6 part of nonionic active agent, 10 parts of hydrogenated vegetable oil, 2.5 parts of cationic lubricant, 13 parts of coupling agent, 2.4 parts of preservative and 0.03 part of defoaming agent.
Comparative example 7 superfine electronic yarn impregnating compound and preparation method thereof
The comparative example differs from example 4 in that the preservative used is 35-40% by mass of formaldehyde.
Example 5-8 an ultra-fine electronic yarn treating compound and a method for preparing the same
The compositions and amounts of the ultra-fine electronic yarn size described in examples 5-8 are shown in Table 2.
TABLE 2
Figure BDA0002671420550000071
The preparation method of the superfine electronic yarn impregnating compound comprises the following steps:
(1) mixing the starch with the formula amount and water, stirring, heating at 96 ℃ and keeping the temperature for 30min, and cooling to 76 ℃ to obtain a gelatinized starch solution;
(2) mixing the mixed grease, the aliphatic polyamide, the fatty acid ester lubricant, the nonionic active agent, the hydrogenated vegetable oil, the cationic lubricant, the coupling agent, the preservative and the defoaming agent according to the formula ratio, and uniformly stirring to obtain the aid;
(3) and (3) mixing the auxiliary agent obtained in the step (2) with the gelatinized starch solution obtained in the step (1) for reaction, and forming emulsion after the temperature is stabilized at 60 ℃ to obtain the superfine electronic yarn impregnating compound.
Comparative example 8 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 8 in that the starch is only starch HR.
Comparative example 9 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 8 in that the starch is only starch HJ.
Comparative example 10 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 8 in that the starch HR is replaced by an unmodified hybrid corn starch with a linear chain of 70%; starch HJ was replaced by an etherified hybrid maize starch with 27% amylose.
Comparative example 11 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 8 in that the weight ratio of starch HR and starch HJ was 40: 20.
Comparative example 12 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 8 in that 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexylformate epoxy resin was used in place of the coupling agent.
Comparative example 13 superfine electronic yarn impregnating compound and preparation method thereof
The difference between the comparative example and example 8 is that the active component comprises 16 parts of mixed grease, 2.4 parts of aliphatic polyamide, 0.6 part of nonionic active agent, 10 parts of hydrogenated vegetable oil, 2.5 parts of cationic lubricant, 13 parts of coupling agent, 2.4 parts of preservative and 0.03 part of defoaming agent.
Comparative example 14 superfine electronic yarn impregnating compound and preparation method thereof
The comparative example differs from example 8 in that the preservative used is 35-40% by mass of formaldehyde.
Example 9-12 an ultra-fine electronic yarn treating agent and method for preparing the same
The compositions and amounts of the ultra-fine electronic yarn size compositions described in examples 9-12 are shown in Table 3.
TABLE 3
Figure BDA0002671420550000091
The preparation method of the superfine electronic yarn impregnating compound comprises the following steps:
(1) mixing the starch with the formula amount and water, stirring, heating at 96 ℃ and keeping the temperature for 30min, and cooling to 76 ℃ to obtain a gelatinized starch solution;
(2) mixing the mixed grease, the aliphatic polyamide, the fatty acid ester lubricant, the nonionic active agent, the hydrogenated vegetable oil, the cationic lubricant, the coupling agent, the preservative and the defoaming agent according to the formula ratio, and uniformly stirring to obtain the aid;
(3) and (3) mixing the auxiliary agent obtained in the step (2) with the gelatinized starch solution obtained in the step (1) for reaction, and forming emulsion after the temperature is stabilized at 60 ℃ to obtain the superfine electronic yarn impregnating compound.
Comparative example 15 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 12 in that the starch is only starch HR.
Comparative example 16 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 12 in that the starch is only starch HJ.
Comparative example 17 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 12 in that the starch HR is replaced by an unmodified hybrid corn starch with an amylose content of 70%; starch HJ was replaced by an etherified hybrid maize starch with 27% amylose.
Comparative example 18 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 12 in that the weight ratio of starch HR and starch HJ was 30: 20.
Comparative example 19 superfine electronic yarn impregnating compound and preparation method thereof
This comparative example differs from example 12 in that 3, 4-epoxycyclohexylmethyl-3, 4-epoxycyclohexylformate epoxy resin is used in place of the coupling agent.
Comparative example 20 superfine electronic yarn impregnating compound and preparation method thereof
The present comparative example differs from example 12 in that the active ingredient contains 16 parts of mixed oil and fat, 2.4 parts of aliphatic polyamide, 0.6 part of nonionic active agent, 10 parts of hydrogenated vegetable oil, 2.5 parts of cationic lubricant, 13 parts of coupling agent, 2.4 parts of preservative, and 0.03 part of defoaming agent.
Comparative example 21 superfine electronic yarn impregnating compound and preparation method thereof
The comparative example differs from example 12 in that the preservative used is 35-40% by mass of formaldehyde.
Experimental example 1
The ultra-fine electronic yarn sizing agents prepared in examples 1 to 12 were subjected to a laboratory test for physical and chemical properties, in which viscosity was measured by means of a Bohler viscometer (40. + -. 0.5 ℃ C.), film strength of the sizing agent was measured by means of a burst tester, and the time of occurrence of rottenness and mildew was observed under the conditions of 40. + -. 0.5 ℃ C and a humidity of 80 to 85% for an anticorrosion effect test. The results are shown in Table 4 below.
TABLE 4
Figure BDA0002671420550000101
Figure BDA0002671420550000111
As can be seen from the above table, the viscosity of the impregnating compound prepared by the invention is between 8.0 and 8.4cps, the range of the very difference is 0.4cps, the pH value is between 5.32 and 5.60, and the range of the very difference is 0.028, which shows that the impregnating compound has good viscosity and pH value stability, meanwhile, the film strength is 175-205KPa, and the mildew time is more than 24h, which shows that the impregnating compound prepared by the invention has high film forming strength and excellent anticorrosion effect.
In order to further verify the technical effects of the present invention, the impregnating agents prepared in comparative examples 5 to 7, comparative examples 12 to 14 and comparative examples 19 to 21 were subjected to film strength and corrosion prevention effect tests, and the results are shown in table 5.
TABLE 5
Figure BDA0002671420550000112
Figure BDA0002671420550000121
As can be seen from the data in the table, compared with the conventional formaldehyde aqueous solution as a preservative, the preservative FS14D adopted in the impregnating compound disclosed by the invention can participate in the reaction of other components of the impregnating compound while improving the corrosion resistance, so that the bundling effect of the impregnating compound is optimized, and the film forming strength of the impregnating compound is improved. Meanwhile, the film forming strength of the prepared impregnating compound is obviously reduced when the dosage of the coupling agent and each component in the impregnating compound is changed, which shows that the dosage of the coupling agent and each component in the impregnating compound has influence on the film forming strength of the impregnating compound.
Experimental example two
The related technical indexes of the D450 (monofilament diameter of 4 μm) ultrafine glass fiber yarns drawn under the same process conditions by using the ultrafine electronic yarn impregnating agents prepared in examples 1 to 4 and comparative examples 1 to 7 are shown in Table 6.
TABLE 6
Figure BDA0002671420550000122
Figure BDA0002671420550000131
The data in the table show that the impregnating compound prepared by the invention can effectively avoid the migration phenomenon of the inner layer and the outer layer, the broken fiber rate of the glass fiber is reduced, the hairiness rate is obviously reduced, the product quality is greatly improved, the product rate is more than 92%, and when the weight ratio of the starch HR to the starch HJ in the impregnating compound is 37:18, the prepared impregnating compound has better performance. Meanwhile, the change of the type and the proportion of the starch and the dosage of each component are found to have influence on the performance of the impregnating compound.
The related technical indexes of the ultrafine glass fiber yarns having a filament diameter of 3.81 μm, which were drawn under the same process conditions using the ultrafine electronic yarn sizes prepared in examples 5 to 8 and comparative examples 8 to 14, are shown in Table 7.
TABLE 7
Figure BDA0002671420550000132
Figure BDA0002671420550000141
The data in the table show that the impregnating compound prepared by the invention can effectively avoid the migration phenomenon of the inner layer and the outer layer, the broken fiber rate of the glass fiber is reduced, the hairiness rate is obviously reduced, the product quality is greatly improved, the product rate is over 90 percent, and when the weight ratio of the starch HR to the starch HJ in the impregnating compound is 4:1, the prepared impregnating compound has better performance. Meanwhile, the change of the type and the proportion of the starch and the dosage of each component are found to have influence on the performance of the impregnating compound.
The related technical indexes of the ultrafine glass fiber yarns having a filament diameter of 3.90 μm, which were drawn under the same process conditions using the ultrafine electronic yarn sizes prepared in examples 9 to 12 and comparative examples 15 to 21, are shown in Table 8.
TABLE 8
Figure BDA0002671420550000142
Figure BDA0002671420550000151
The data in the table show that the impregnating compound prepared by the invention can effectively avoid the migration phenomenon of the inner layer and the outer layer, the broken fiber rate of the glass fiber is reduced, the hairiness rate is obviously reduced, the product quality is greatly improved, the product rate is more than 91%, and when the weight ratio of the starch HR to the starch HJ in the impregnating compound is 1:1, the prepared impregnating compound has better performance. Meanwhile, the change of the type and the proportion of the starch and the dosage of each component are found to have influence on the performance of the impregnating compound.
In conclusion, the novel starch HR and the starch HJ are compounded to form a new molecular structure, and the effective combination degree of other auxiliary agents between the starch and the surface of the glass fiber is changed, so that the combination of the impregnating compound and the surface of the superfine yarn glass fiber is firmer, and the performance of the impregnating compound is effectively improved. The prepared sizing agent can be used for producing superfine electronic yarns with the monofilament diameter of 3.81-4 microns, the phenomenon of migration of the inner layer and the outer layer can be effectively avoided, the breakage rate of the prepared glass fiber is reduced, the hairiness rate is obviously reduced, the product quality is greatly improved, and the product rate is over 90 percent.
Meanwhile, the preservative FS14D adopted in the impregnating compound can participate in the reaction of other components of the impregnating compound while improving the corrosion resistance, optimize the bundling effect of the impregnating compound and improve the film forming strength of the impregnating compound.
The impregnating compound eliminates the harm of formaldehyde volatilization to human bodies, prolongs the time effect of the preservative, can prepare 4 tons of impregnating compound per tank (the maximum amount of the conventional formaldehyde preservative is 2 tons), and improves the production efficiency.
The present invention has been further described with reference to specific embodiments, which are only exemplary and do not limit the scope of the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (10)

1. The superfine electronic yarn impregnating compound is characterized by comprising 6.5-7 mass percent of superfine electronic yarn impregnating compound active components and the balance of water;
the superfine electronic yarn impregnating compound comprises the following active components in parts by weight: 44-65.7 parts of starch, 9-15 parts of mixed grease, 0.8-2.2 parts of aliphatic polyamide, 2.6-5.1 parts of fatty acid ester lubricant, 0.7-2.1 parts of nonionic active agent, 5.2-9.6 parts of hydrogenated vegetable oil, 2.8-5.1 parts of cationic lubricant, 6.8-12.2 parts of coupling agent, 0.7-2.3 parts of preservative and 0.01-0.04 part of defoaming agent;
the starch consists of starch HR and starch HJ.
2. The electronic ultrafine yarn size as claimed in claim 1, wherein the weight ratio of starch HR to starch HJ in the starch is 31-43: 15-21.
3. The electronic ultrafine yarn size as recited in claim 1, wherein the weight ratio of starch HR to starch HJ in said starch is 38.2-51.2: 8.8-14.5.
4. The electronic ultrafine yarn size as claimed in claim 1, wherein the weight ratio of starch HR to starch HJ in the starch is 22-31: 22-31.
5. The electronic sizing material for ultra-fine yarns as claimed in claim 1, wherein the mixed grease is mixed grease AM.
6. The electronic ultrafine yarn size as recited in claim 1, wherein said cationic lubricant is E-SO.
7. The electronic ultrafine yarn size as recited in claim 1, wherein the preservative is FS-14D.
8. The electronic sizing material for ultra-fine yarn as recited in claim 1, wherein said coupling agent is a silane coupling agent.
9. The method for preparing the ultra-fine electronic yarn size as claimed in any one of claims 1 to 8, comprising the steps of:
(1) mixing the starch with the formula amount and water, stirring, heating, preserving heat and cooling to obtain a gelatinized starch solution;
(2) mixing the mixed grease, the aliphatic polyamide, the fatty acid ester lubricant, the nonionic active agent, the hydrogenated vegetable oil, the cationic lubricant, the coupling agent, the preservative and the defoaming agent according to the formula ratio, and uniformly stirring to obtain the aid;
(3) mixing the auxiliary agent obtained in the step (2) with the gelatinized starch solution obtained in the step (1) for reaction, and forming an emulsion after the temperature is stable to obtain the superfine electronic yarn impregnating compound;
in the step (1), the heating and heat preservation is carried out at 96 ℃ for 30 min; the temperature is reduced to 76 ℃;
the temperature after the temperature stabilization in the step (3) is 60 ℃.
10. The use of the ultra fine electronic yarn size as claimed in any one of claims 1 to 8 in the production of ultra fine glass fiber electronic yarn.
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CN117303754A (en) * 2023-09-21 2023-12-29 清远忠信世纪电子材料有限公司 Glass fiber antistatic impregnating compound and preparation method thereof
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