CN113527736A - High-permeability insulating glass fiber resin plate and preparation method thereof - Google Patents

High-permeability insulating glass fiber resin plate and preparation method thereof Download PDF

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Publication number
CN113527736A
CN113527736A CN202110863170.2A CN202110863170A CN113527736A CN 113527736 A CN113527736 A CN 113527736A CN 202110863170 A CN202110863170 A CN 202110863170A CN 113527736 A CN113527736 A CN 113527736A
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prepared
glass fiber
resin plate
parts
agent
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张宗权
何辉春
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Huizhou Zongsheng Electronic Material Co ltd
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Huizhou Zongsheng Electronic Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/02—Coating on the layer surface on fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00—Coating on the layer surface
    • B32B2255/26—Polymeric coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/101—Glass fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/206—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B32B2307/7145—Rot proof, resistant to bacteria, mildew, mould, fungi
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    • C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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    • C08K5/00—Use of organic ingredients
    • C08K5/49—Phosphorus-containing compounds
    • C08K5/51—Phosphorus bound to oxygen
    • C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
    • C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
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Abstract

The invention discloses a high-permeability insulating glass fiber resin plate and a preparation method thereof, wherein the glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, and the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material; the reinforcing material is continuous glass fiber cloth; the glue solution is prepared from a main adhesive and a curing agent according to the mass ratio of (3-4): 1.2-1.3; the main binder is prepared from the following raw materials, by weight, 50-60 parts of epoxy resin and 3-9 parts of an auxiliary agent; the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine; the auxiliary agent is prepared from the following raw materials in parts by weight, 2-4 parts of a flame retardant and 1-5 parts of an antibacterial agent. The invention adds the antibacterial agent and the flame retardant, the antibacterial property of the product can be improved by adding the antibacterial agent, the flame retardant can be improved by adding the flame retardant, the application field of the product is further widened, the service life of the product is prolonged, and the use cost is reduced.

Description

High-permeability insulating glass fiber resin plate and preparation method thereof
Technical Field
The invention relates to the technical field of plate preparation, in particular to a high-permeability insulating glass fiber resin plate and a preparation method thereof.
Background
The glass fiber is an inorganic non-metallic material with excellent performance, has the advantages of good insulating property, high mechanical strength and strong heat and corrosion resistance, and the mechanical strength and the insulating property of the product can be greatly improved by adding the glass fiber into the resin plate.
The epoxy resin is common organic resin in the market, contains epoxy group, and can be subjected to ring opening and further curing and crosslinking after a substance containing active hydrogen is added, so that the purpose of curing and crosslinking is achieved. The glue solution for the plate on the market at present is various in types, and part of the glue solution also contains substances harmful to human bodies, such as phenol, formaldehyde and the like, so that the product is harmful to the environment and the health of the human bodies.
Disclosure of Invention
The invention aims to provide a high-permeability insulating glass fiber resin plate and a preparation method thereof, and aims to solve the problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme: a high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to the mass ratio of (3-4): 1.2-1.3;
the main binder is prepared from the following raw materials, by weight, 50-60 parts of epoxy resin and 3-9 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
Furthermore, the auxiliary agent is prepared from the following raw materials in parts by weight, 2-4 parts of a flame retardant and 1-5 parts of an antibacterial agent.
Furthermore, the antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
Further, the flame retardant is prepared from triethylamine, phenylphosphonic dichloride, triethylamine hydrochloride, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, diaminodiphenylmethane and a catalyst.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, and carrying out reflux heating to obtain a mixture A;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, and obtaining an antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling, adding a toluene solution of phenylphosphonic dichloride, then starting to heat, carrying out reflux heating, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, a solvent and a catalyst, carrying out reflux heating, and obtaining an auxiliary agent after the reaction is finished;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
and taking a plurality of layers of prepreg, cutting, stacking and compounding by hot pressing to obtain the resin plate.
Further, the concrete steps are as follows,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, refluxing and heating at 70-80 ℃ for 2-3h to obtain a mixture A;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, reacting for 4.8-5.2h, and obtaining an antibacterial agent after the reaction is finished;
the added auxiliary agent contains an antibacterial agent and a flame retardant, wherein the main raw materials of the antibacterial agent are phenol, trichlorophenol, sodium hydroxide and 2-amino-5-alkyl-1, 3, 4-thiadiazole, wherein the phenol and the trichlorophenol generate o-hydroxybenzaldehyde under the action of alkaline solution sodium hydroxide, then the 2-amino-5-alkyl-1, 3, 4-thiadiazole is added into the obtained o-hydroxybenzaldehyde, and the antibacterial agent can be obtained after reaction, so that the antibacterial performance of the product can be improved, the influence of fungus substances on the product in a humid environment can be reduced, and the service life of the product can be further prolonged.
The raw materials are selected from phenol, and the phenol is in a category 3 carcinogen list, so that in order to reduce phenol residue, the mass ratio of the added trichloromethane to the phenol is limited to be 0.9-1:1, the phenol can be ensured to completely participate in the reaction, and the lowest phenol content in the product is further ensured.
This application participates in the reaction through adding excessive trichloromethane, has reduced the residue of phenol, can produce certain negative effects, leads to remaining a large amount of trichloromethane, and in normal preparation process, the mode that adopts the heating evaporation goes out remaining trichloromethane evaporation, and then guarantees that the content of trichloromethane is minimum in the product, but trichloromethane has certain toxicity, causes harm to environment and human body.
(3) Dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling to 1-2 ℃, adding a toluene solution of phenylphosphonyl dichloride, then starting to heat, carrying out reflux heating to 30-35 ℃, reacting for 4.5h, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, a solvent and a catalyst, heating to 150 ℃ and 160 ℃, and removing the solvent to obtain an auxiliary agent;
phenol and trichloromethane are used in the process of preparing the antibacterial agent, the obtained o-hydroxybenzaldehyde is used as a main product, and a byproduct p-hydroxybenzaldehyde can be generated.
The added 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide contains a P-H bond, so that the flame retardant with high stability and strong flame retardant property can be used for life, and the auxiliary agent prepared by the method contains a small amount of chloride, does not contain toxic substances such as phenol, trichloromethane and the like, so that the use safety and the service life of the product are improved.
S2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
and taking a plurality of layers of prepreg, cutting, stacking and compounding by hot pressing to obtain the resin plate.
Further, the solvent used in step S1 is dimethyl sulfoxide.
Further, the molar ratio of the chloroform to the phenol added in step S1 is 3-4: 1.
Further, step S3, the hot pressing temperature is 140-2The time is 1.8-2.2h, and the vacuum degree is 740-750 mmHg.
Compared with the prior art, the invention has the following beneficial effects: the glass fiber is an inorganic non-metallic material with excellent performance, has the advantages of good insulating property, high mechanical strength and strong heat and corrosion resistance, and the mechanical strength and the insulating property of the product can be greatly improved by adding the glass fiber into the resin plate.
The main component of the glue solution used in the application is epoxy resin, the epoxy resin contains epoxy groups, and after a substance containing active hydrogen is added, the epoxy resin can be subjected to ring opening to generate curing crosslinking, so that the purpose of curing crosslinking is achieved.
The application is on the basis of epoxy resin, the auxiliary agent is added, the auxiliary agent contains the antibacterial agent and the flame retardant, the antibacterial performance of the product can be improved by adding the antibacterial agent, the flame retardant performance of the product can be improved by adding the flame retardant, the use field of the product is further widened, the service life of the product is prolonged, and the use cost is reduced.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to the mass ratio of 3: 1.2 mixing;
the main binder is prepared from the following raw materials in parts by weight, 50 parts of epoxy resin and 3 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
The auxiliary agent is prepared from the following raw materials in parts by weight, 2 parts of flame retardant and 1 part of antibacterial agent.
The antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
The flame retardant is prepared from triethylamine, phenylphosphonic dichloride, triethylamine hydrochloride, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, diaminodiphenylmethane and a catalyst.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, heating under reflux at 70 ℃ for 2h, wherein the molar ratio of trichloromethane to phenol is 3:1, and obtaining a mixture A;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, reacting for 4.8h, and obtaining the antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling to 1 ℃, adding a toluene solution of phenylphosphonyl dichloride, then starting to heat, refluxing and heating to 30 ℃, reacting for 4.5 hours, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, dimethyl sulfoxide and a catalyst, heating to 150 ℃, and removing the solvent to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
taking a plurality of layers of prepreg, cutting, overlapping, hot-pressing and compounding, wherein the hot-pressing temperature is 140 ℃, and the pressure is 10kgf/cm2Keeping the vacuum degree at 740mmHg for 1.8h to obtain a resin plate;
example 2
A high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to the mass ratio of 3.5: 1.25 mixing;
the main binder is prepared from the following raw materials in parts by weight, 55 parts of epoxy resin and 6 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
The auxiliary agent is prepared from the following raw materials in parts by weight, 3 parts of a flame retardant and 3 parts of an antibacterial agent.
The antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
The flame retardant is prepared from triethylamine, phenylphosphonic dichloride, triethylamine hydrochloride, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, diaminodiphenylmethane and a catalyst.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing the trichloromethane and the phenol at a molar ratio of 3.5:1, adding sodium hydroxide, heating under reflux at 75 ℃ for 2.5 hours to obtain a mixture A;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the solution into the mixture A, adding p-toluenesulfonic acid, stirring for 5 hours, and obtaining an antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling to 1.5 ℃, adding a toluene solution of phenylphosphonyl dichloride, then starting to heat, carrying out reflux heating to 30-35 ℃, reacting for 4.5h, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, dimethyl sulfoxide and a catalyst, heating to 155 ℃, and removing the solvent to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
taking a plurality of layers of prepreg, cutting, overlapping, hot-pressing and compounding, wherein the hot-pressing temperature is 150 ℃, and the pressure is 13kgf/cm2The time is 2h, the vacuum degree is 745mmHg, and a plate is obtained.
Example 3
A high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to a mass ratio of 4: 1.3 mixing;
the main binder is prepared from the following raw materials in parts by weight, 60 parts of epoxy resin and 9 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
The auxiliary agent is prepared from the following raw materials in parts by weight, 4 parts of flame retardant and 5 parts of antibacterial agent.
The antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
The flame retardant is prepared from triethylamine, phenylphosphonic dichloride, triethylamine hydrochloride, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, diaminodiphenylmethane and a catalyst.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, heating under reflux at 80 ℃ for 2-3h, and obtaining a mixture A, wherein the molar ratio of the trichloromethane to the phenol is 4: 1;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, reacting for 5.2h, and obtaining the antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling to 2 ℃, adding a toluene solution of phenylphosphonyl dichloride, then starting to heat, refluxing and heating to 30-35 ℃, reacting for 4.5 hours, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, dimethyl sulfoxide and a catalyst, heating to 160 ℃, and removing the solvent to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
taking a plurality of layers of prepregs, cutting, overlapping, hot-pressing and compounding, wherein the hot-pressing temperature is 160 ℃, and the pressure is 15kgf/cm2The time is 2.2h, the vacuum degree is 750mmHg, and a plate is obtained.
Comparative example 1
A high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to a mass ratio of 4: 1.3 mixing;
the main binder is prepared from the following raw materials in parts by weight, 60 parts of epoxy resin and 9 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
The auxiliary agent is prepared from the following raw materials in parts by weight, 4 parts of flame retardant and 5 parts of antibacterial agent.
The antibacterial agent is ethyl vanillin compound and acylaniline compound.
The flame retardant is antimony trioxide, magnesium hydroxide and tricresyl phosphate.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
mixing the antibacterial agent ethyl vanillin compounds and acylaniline compounds with flame retardant antimony trioxide, magnesium hydroxide and tricresyl phosphate, and stirring to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
taking a plurality of layers of prepregs, cutting, overlapping, hot-pressing and compounding, wherein the hot-pressing temperature is 160 ℃, and the pressure is 15kgf/cm2The time is 2.2h, the vacuum degree is 750mmHg, and a plate is obtained.
Comparative example 2
A high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to a mass ratio of 4: 1.3 mixing;
the main binder is prepared from the following raw materials in parts by weight, 60 parts of epoxy resin and 9 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
The auxiliary agent is prepared from the following raw materials in parts by weight, 4 parts of flame retardant and 5 parts of antibacterial agent.
The antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
The flame retardant is antimony trioxide, magnesium hydroxide and tricresyl phosphate.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, heating under reflux at 80 ℃ for 2-3h, and obtaining a mixture A, wherein the molar ratio of the trichloromethane to the phenol is 4: 1;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, reacting for 5.2h, and obtaining the antibacterial agent after the reaction is finished;
(3) adding flame retardant antimony trioxide, magnesium hydroxide and tricresyl phosphate into the obtained antibacterial agent, and uniformly stirring to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
taking a plurality of layers of prepreg, cutting, overlapping, hot-pressing and compounding, wherein the hot-pressing temperature is 160 ℃,the pressure was 15kgf/cm2The time is 2.2h, the vacuum degree is 750mmHg, and a plate is obtained.
Comparative example 3
A high-permeability insulating glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two surfaces of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to a mass ratio of 4: 1.3 mixing;
the main binder is prepared from the following raw materials in parts by weight, 60 parts of epoxy resin and 9 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
The auxiliary agent is prepared from the following raw materials in parts by weight, 4 parts of flame retardant and 5 parts of antibacterial agent.
The antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
The flame retardant is prepared from triethylamine, phenylphosphonic dichloride, triethylamine hydrochloride, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, diaminodiphenylmethane and a catalyst.
A preparation method of a high-permeability insulating glass fiber resin plate comprises the following steps,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, heating under reflux at 80 ℃ for 2-3h, and obtaining a mixture A, wherein the molar ratio of the trichloromethane to the phenol is 1: 1;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, reacting for 5.2h, and obtaining the antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling to 2 ℃, adding a toluene solution of phenylphosphonyl dichloride, then starting to heat, refluxing and heating to 30-35 ℃, reacting for 4.5 hours, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, dimethyl sulfoxide and a catalyst, heating to 160 ℃, and removing the solvent to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
taking a plurality of layers of prepregs, cutting, overlapping, hot-pressing and compounding, wherein the hot-pressing temperature is 160 ℃, and the pressure is 15kgf/cm2The time is 2.2h, the vacuum degree is 750mmHg, and a plate is obtained.
Experiment of
Comparative examples 1, 2 and 3 were set up with example 3 as a control, wherein a control experiment was performed using the conventional antibacterial agent and flame retardant in comparative example 1, the conventional flame retardant in comparative example 2 and no excess of chloroform in comparative example 3.
The glue solutions of the samples of example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 were subjected to antibacterial and flame retardant property tests, and the results were as follows,
experimental group Antibacterial Property (%) Flame retardant Properties (%)
Example 1 95 92
Example 2 96 91
Example 3 96 92
Comparative example 1 92 87
Comparative example 2 91 86
Comparative example 3 89 81
Watch 1
The phenol residue in the glue solutions of the samples of example 1, example 2, example 3, comparative example 2 and comparative example 3 was measured, and the results were as follows,
experimental group Phenol (mg/kg)
Example 1 ＜0.1
Example 2 ＜0.1
Example 3 ＜0.1
Comparative example 2 ＜0.1
Comparative example 3 0.5
Watch two
The conventional antibacterial agent and the conventional flame retardant are used in the comparative example 1, and the flame retardant and the antibacterial performance in the comparative example 1 are basically the same as those in the examples 1, 2 and 3, so that the examples 1, 2 and 3 have more excellent flame retardant and antibacterial effects, and the content of residual phenol is reduced to the minimum, thereby ensuring the safety of the environment and the human body.
The conventional flame retardant is used in the comparative example 2, and the flame retardant and antibacterial performance of the comparative example 2 is lower compared with that of the examples 1, 2 and 3, which shows that the examples 1, 2 and 3 have excellent antibacterial and flame retardant performances.
In comparative example 3, the addition of excessive trichloromethane leads to lower antibacterial performance and flame retardant performance of comparative example 3 compared with examples 1, 2 and 3 and higher residual phenol content compared with examples 1, 2 and 3, which shows that the flame retardant performance and antibacterial performance of products are better and the residual phenol content is lower when a series of treatments are carried out in examples 1, 2 and 3.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A high-transparency insulating glass fiber resin plate is characterized in that: the glass fiber resin plate is prepared by hot-pressing and compounding a plurality of layers of prepreg, wherein the prepreg is mainly prepared by coating glue solution on two sides of a reinforcing material;
the reinforcing material is continuous glass fiber cloth;
the glue solution is prepared from a main adhesive and a curing agent according to the mass ratio of (3-4): 1.2-1.3;
the main binder is prepared from the following raw materials, by weight, 50-60 parts of epoxy resin and 3-9 parts of an auxiliary agent;
the curing agent is prepared by mixing ethylenediamine, diethylenetriamine and triethylene tetramine.
2. The high-permeability insulating glass fiber resin plate as claimed in claim 1, wherein: the auxiliary agent is prepared from the following raw materials in parts by weight, 2-4 parts of a flame retardant and 1-5 parts of an antibacterial agent.
3. The high-permeability insulating glass fiber resin plate as claimed in claim 2, wherein: the antibacterial agent is prepared from phenol, trichloromethane, sodium hydroxide, 2-amino-5-alkyl-1, 3, 4-thiadiazole and p-toluenesulfonic acid.
4. The high-permeability insulating glass fiber resin plate as claimed in claim 2, wherein: the flame retardant is prepared from triethylamine, phenylphosphonic dichloride, triethylamine hydrochloride, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, diaminodiphenylmethane and a catalyst.
5. A preparation method of a high-permeability insulating glass fiber resin plate is characterized by comprising the following steps: the steps are as follows,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, and carrying out reflux heating to obtain a mixture A;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, and obtaining an antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling, adding a toluene solution of phenylphosphonic dichloride, then starting to heat, carrying out reflux heating, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, a solvent and a catalyst, carrying out reflux heating, and obtaining an auxiliary agent after the reaction is finished;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
and taking a plurality of layers of prepreg, cutting, stacking and compounding by hot pressing to obtain the resin plate.
6. The method for preparing a high-permeability insulating glass fiber resin plate as claimed in claim 5, wherein the method comprises the following steps: the specific steps are as follows,
s1, preparation of an auxiliary agent:
(1) putting phenol and trichloromethane into a closed container, mixing, adding sodium hydroxide, refluxing and heating at 70-80 ℃ for 2-3h to obtain a mixture A;
(2) dissolving 2-amino-5-alkyl-1, 3, 4-thiadiazole in ethanol, adding the mixture into the mixture A, adding p-toluenesulfonic acid, stirring, reacting for 4.8-5.2h, and obtaining an antibacterial agent after the reaction is finished;
(3) dissolving phenylphosphonic dichloride in a toluene solution for later use; dissolving 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a toluene solution for later use;
(4) adding triethylamine into the obtained antibacterial agent, cooling to 1-2 ℃, adding a toluene solution of phenylphosphonyl dichloride, then starting to heat, carrying out reflux heating to 30-35 ℃, reacting for 4.5h, adding a triethylamine hydrochloride solution after the reaction is finished, filtering, adding a toluene solution of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, charging nitrogen, adding diaminodiphenylmethane, a solvent and a catalyst, heating to 150 ℃ and 160 ℃, and removing the solvent to obtain an auxiliary agent;
s2, preparation of glue solution: mixing epoxy resin and an auxiliary agent to obtain a main binder, heating, uniformly stirring, and adding a curing agent to obtain a glue solution;
s3, coating the obtained glue solution on two sides of the reinforced material, and curing to form a prepreg;
and taking a plurality of layers of prepreg, cutting, stacking and compounding by hot pressing to obtain the resin plate.
7. The method for preparing a high-permeability insulating glass fiber resin plate as claimed in claim 6, wherein the method comprises the following steps: the solvent used in step S1 is dimethyl sulfoxide.
8. The method for preparing a high-permeability insulating glass fiber resin plate as claimed in claim 6, wherein the method comprises the following steps: the molar ratio of chloroform to phenol added in step S1 is 3-4: 1.
9. The method for preparing a high-permeability insulating glass fiber resin plate as claimed in claim 6, wherein the method comprises the following steps: step S3, the hot pressing temperature is 140-160 ℃, and the pressure is 10-15kgf/cm2The time is 1.8-2.2h, and the vacuum degree is 740-750 mmHg.
CN202110863170.2A 2021-07-29 2021-07-29 High-permeability insulating glass fiber resin plate and preparation method thereof Pending CN113527736A (en)

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