CN113061223B - Preparation method of epoxy soybean oil modified resin and method for preparing paper-based copper-clad plate - Google Patents
Preparation method of epoxy soybean oil modified resin and method for preparing paper-based copper-clad plate Download PDFInfo
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- CN113061223B CN113061223B CN202110308902.1A CN202110308902A CN113061223B CN 113061223 B CN113061223 B CN 113061223B CN 202110308902 A CN202110308902 A CN 202110308902A CN 113061223 B CN113061223 B CN 113061223B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
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- 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
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- 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
- B32B37/08—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the cooling method
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- 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
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- 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
- B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
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- 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
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Abstract
The application provides a preparation method of epoxidized soybean oil modified resin and a method for preparing a paper-based copper-clad plate, and solves the technical problems that in the prior art, an adhesive cannot simultaneously meet the requirements of flame retardant property and small environmental pollution. According to the preparation method of the nitrogen-containing epoxy soybean oil modified resin, the material containing the amine compound is added in the reaction of the epoxy soybean oil modified resin, and the amine-containing compound contains the specific nitrogen element, so that the nitrogen-containing epoxy soybean oil modified resin has excellent flame retardant property, and therefore, when the nitrogen-containing epoxy soybean oil modified resin is used as a main material for preparing an adhesive, the fire resistance of the adhesive and the curing property of a waterproof agent are enhanced, the flame retardant effect is achieved, and the amine-containing compound does not contain any halogen element, so that the environmental pollution is reduced.
Description
Technical Field
The application relates to the technical field of paper-based copper-clad plates, in particular to a preparation method of epoxidized soybean oil modified resin and a method for preparing the paper-based copper-clad plate.
Background
With the development of the building industry, the paper-based phenolic aldehyde copper-clad plate is the largest product in demand among copper-clad plate products, and is mainly used for household electrical appliances such as sound equipment, VTR, televisions and the like. The paper-based phenolic aldehyde copper-clad plate not only has proper performance price, can be produced in quantity, but also is easy to process. Therefore, the condition is always good for a long time. However, in recent years, as the size and density of home electric appliances have been reduced, the substrates for home electric appliances are required to have the same level of characteristics as those of industrial electronic products. Under such circumstances, the modified phenol resin has been improved in electrical characteristics, high heat resistance, low material cost, and the like. In the production and use processes of the paper-based copper-clad plate, safety and reliability are important marks of product quality, and the flame retardance must reach V-0 level specified by UL standard.
At present, with the international requirements on flame-retardant and environment-friendly materials becoming stricter, halogen-containing compounds can release toxic substances in the combustion process, which affects the health of people and pollutes the environment.
Disclosure of Invention
In view of the above, the application provides a preparation method of epoxidized soybean oil modified resin and a preparation method of a paper-based copper-clad plate, which solve the technical problems that in the prior art, an adhesive cannot simultaneously meet the requirements of flame retardant property and small environmental pollution.
For the purpose of making the present application more apparent, its objects, technical means and advantages will be further described in detail with reference to the accompanying drawings.
According to one aspect of the present application, the present application provides a method for preparing a nitrogen-containing epoxy soybean oil modified resin, comprising the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under the alkaline condition, adding an amine compound and phenolic resin into a reaction kettle for polycondensation; and
step S103: adding a gelatinizing agent into a reaction kettle, gelatinizing for 3-10 minutes at 160-200 ℃, and then performing vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
In an embodiment of the present application, in step S102, the amine compound is melamine.
In an embodiment of the present invention, in step S102, a ratio of the mass of the melamine to a sum of the mass of the melamine, the epoxy soybean oil after the epoxy ring opening, the bisphenol a, the cardanol, and the phenol resin is 2 to 5%.
In an embodiment of the present application, in step S102, the ratio of the mass of the melamine to the sum of the masses of the melamine, the epoxidized soybean oil after the ring opening of the epoxy group, the bisphenol a, the cardanol, and the phenol resin is 3%.
In an embodiment of the present application, in step S102, the alkaline condition is: a sodium hydroxide solution having a pH of 7.5 to 8.2.
In an embodiment of the present application, in step S102, the phenolic resin includes: phenol and formaldehyde.
As a second aspect of the application, the application provides a method for preparing a paper-based copper-clad plate by adopting nitrogen-containing epoxy soybean oil modified resin, which comprises the following steps:
step S201: dissolving nitrogen-containing epoxy soybean oil modified resin and epoxy resin in a solvent, and fully stirring to generate a mixed solution, wherein the nitrogen-containing epoxy soybean oil modified resin is prepared by the preparation method of the nitrogen-containing epoxy soybean oil modified resin;
step S202: curing the mixed solution to generate a resin glue solution;
step S203: coating the resin glue solution on two sides of the wood pulp paper, baking to remove the solvent, and then dip-coating the resin glue solution on two sides to obtain a sizing sheet;
step S204: and overlapping a plurality of the sizing material sheets and the sizing foil together, putting the mixture between two steel plates, and carrying out hot pressing and cooling to obtain the nitrogenous epoxy soybean oil modified resin for preparing the paper-based copper-clad plate.
In an embodiment of the present application, the solvent comprises methanol.
According to the preparation method of the nitrogen-containing epoxy soybean oil modified resin, the material containing the amine compound is added in the reaction of the epoxy soybean oil modified resin, and the amine-containing compound contains the specific nitrogen element, so that the nitrogen-containing epoxy soybean oil modified resin has excellent flame retardant property, and therefore, when the nitrogen-containing epoxy soybean oil modified resin is used as a main material for preparing an adhesive, the fire resistance of the adhesive and the curing property of a waterproof agent are enhanced, the flame retardant effect is achieved, and the amine-containing compound does not contain any halogen element, so that the environmental pollution is reduced.
Drawings
FIG. 1 is a schematic flow chart illustrating a method for preparing a nitrogen-containing epoxy soybean oil modified resin according to an embodiment of the present disclosure;
fig. 2 is a schematic flow chart of a method for preparing a paper-based copper-clad plate by using nitrogen-containing epoxy soybean oil modified resin according to an embodiment of the present application.
Detailed Description
In the description of the present application, "plurality" means at least two, e.g., two, three, etc., unless explicitly specifically limited otherwise. All directional indicators in the embodiments of the present application (such as upper, lower, left, right, front, rear, top, bottom … …) are only used to explain the relative positional relationship between the components, the movement, etc. in a particular posture (as shown in the drawings), and if the particular posture is changed, the directional indicator is changed accordingly. Furthermore, the terms "include" and "have," as well as any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.
Furthermore, reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. It is explicitly and implicitly understood by one skilled in the art that the embodiments described herein can be combined with other embodiments.
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the 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 application.
As a first aspect of the present application, the present application provides a method for preparing a nitrogen-containing epoxy soybean oil modified resin, fig. 1 is a schematic flow chart of a method for preparing a nitrogen-containing epoxy soybean oil modified resin provided in an embodiment of the present application, and as shown in fig. 1, an embodiment of the present application provides a method for preparing a nitrogen-containing epoxy soybean oil modified resin, including the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under the alkaline condition, adding an amine compound and phenolic resin into a reaction kettle for polycondensation; and
step S103: adding a gelatinizing agent into a reaction kettle, gelatinizing for 3-10 minutes at 160-200 ℃, and then performing vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
According to the preparation method of the nitrogen-containing epoxy soybean oil modified resin, the material containing the amine compound is added in the reaction of the epoxy soybean oil modified resin, and the amine-containing compound contains the specific nitrogen element, so that the nitrogen-containing epoxy soybean oil modified resin has excellent flame retardant property, and therefore, when the nitrogen-containing epoxy soybean oil modified resin is used as a main material for preparing an adhesive, the fire resistance of the adhesive and the curing property of a waterproof agent are enhanced, the flame retardant effect is achieved, and the amine-containing compound does not contain any halogen element, so that the environmental pollution is reduced.
The following will describe in detail a method for preparing a nitrogen-containing epoxy soybean oil-modified resin with specific examples.
The first embodiment is as follows:
in this embodiment, in step S102, the amine compound includes melamine, and the phenol resin includes: phenol and formaldehyde. In step S102, the alkaline conditions are: sodium hydroxide solution at pH 7.5.
That is, the preparation method of the nitrogen-containing epoxy soybean oil modified resin provided by this embodiment includes the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under an alkaline condition, adding melamine, formaldehyde and phenol into a reaction kettle for polycondensation, wherein the mass ratio of the melamine to the sum of the mass of the melamine, epoxy soybean oil subjected to epoxy ring opening, bisphenol A, cardanol, formaldehyde and phenol is 2%; and
step S103: adding a gelling agent into a reaction kettle, carrying out gelling reaction for 10 minutes at the temperature of 200 ℃, and then carrying out vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
Example two:
in this embodiment, in step S102, the amine compound includes melamine, and the phenol resin includes: phenol and formaldehyde. In step S102, the alkaline conditions are: sodium hydroxide solution at pH 8.2.
That is, the preparation method of the nitrogen-containing epoxy soybean oil modified resin provided by this embodiment includes the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under an alkaline condition, adding melamine, formaldehyde and phenol into a reaction kettle for polycondensation, wherein the mass ratio of the melamine to the sum of the mass of the melamine, epoxy soybean oil subjected to epoxy ring opening, bisphenol A, cardanol, formaldehyde and phenol is 5%; and
step S103: adding a gelatinizing agent into a reaction kettle, gelatinizing for 3 minutes at 160 ℃, and then carrying out vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
Example three:
in this embodiment, in step S102, the amine compound includes melamine, and the phenol resin includes: phenol and formaldehyde. In step S102, the alkaline conditions are: sodium hydroxide solution at pH 8.
That is, the preparation method of the nitrogen-containing epoxy soybean oil modified resin provided by this embodiment includes the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under an alkaline condition, adding melamine, formaldehyde and phenol into a reaction kettle for polycondensation, wherein the mass ratio of the melamine to the sum of the mass of the melamine, epoxy soybean oil subjected to epoxy ring opening, bisphenol A, cardanol, formaldehyde and phenol is 2%; and
step S103: adding a gelling agent into a reaction kettle, carrying out gelling reaction for 5 minutes at 180 ℃, and then carrying out vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
Example four:
in this embodiment, in step S102, the amine compound includes melamine, and the phenol resin includes: phenol and formaldehyde. In step S102, the alkaline conditions are: sodium hydroxide solution at pH 7.8.
That is, the preparation method of the nitrogen-containing epoxy soybean oil modified resin provided by this embodiment includes the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under an alkaline condition, adding melamine, formaldehyde and phenol into a reaction kettle for polycondensation, wherein the mass ratio of the melamine to the sum of the mass of the melamine, epoxy soybean oil subjected to epoxy ring opening, bisphenol A, cardanol, formaldehyde and phenol is 3%; and
step S103: adding a gelling agent into a reaction kettle, carrying out gelling reaction for 7 minutes at 180 ℃, and then carrying out vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
Example five:
in this embodiment, in step S102, the amine compound includes melamine, and the phenol resin includes: phenol and formaldehyde. In step S102, the alkaline conditions are: sodium hydroxide solution at pH 7.6.
That is, the preparation method of the nitrogen-containing epoxy soybean oil modified resin provided by this embodiment includes the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under an alkaline condition, adding melamine, formaldehyde and phenol into a reaction kettle for polycondensation, wherein the mass ratio of the melamine to the sum of the mass of the melamine, epoxy soybean oil subjected to epoxy ring opening, bisphenol A, cardanol, formaldehyde and phenol is 4%; and
step S103: adding a gelling agent into a reaction kettle, carrying out gelling reaction for 6 minutes at 190 ℃, and then carrying out vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin.
In the first to fifth embodiments, the amine compound in the step S102 is melamine, and the current market price of melamine is about 7400 yuan/ton, and the current market price of brominated epoxy paper is 24000 yuan/ton, so that, compared with the halogen-containing flame-retardant epoxy soybean oil resin, the nitrogen-containing epoxy soybean oil modified resin prepared by modifying epoxy soybean oil with melamine in the present application can reduce the usage amount of 10% brominated epoxy resin when used for preparing a copper-clad plate, thereby effectively reducing the material cost, and being green and environment-friendly.
As a second aspect of the application, the application provides a method for preparing a paper-based copper-clad plate by using nitrogen-containing epoxy soybean oil modified resin, and fig. 2 is a schematic flow diagram of the method for preparing the paper-based copper-clad plate by using nitrogen-containing epoxy soybean oil modified resin provided by an embodiment of the application. As shown in figure 2, the method for preparing the paper-based copper-clad plate by adopting the nitrogen-containing epoxy soybean oil modified resin comprises the following steps:
step S201: dissolving nitrogen-containing epoxy soybean oil modified resin and epoxy resin in a solvent, and fully stirring to generate a mixed solution, wherein the nitrogen-containing epoxy soybean oil modified resin is prepared by adopting the preparation method of the nitrogen-containing epoxy soybean oil modified resin prepared in any one of the first to fifth embodiments;
step S202: curing the mixed solution to generate a resin glue solution;
step S203: coating the resin glue solution on two sides of the wood pulp paper, baking to remove the solvent, and then dip-coating the resin glue solution on two sides to obtain a sizing sheet;
step S204: and overlapping a plurality of the sizing material sheets and the sizing foil together, putting the mixture between two steel plates, and carrying out hot pressing and cooling to obtain the nitrogenous epoxy soybean oil modified resin for preparing the paper-based copper-clad plate.
The application provides a method for preparing a paper-based copper-clad plate by adopting nitrogen-containing epoxy soybean oil modified resin, the paper-based copper-clad plate is prepared by adopting the nitrogen-containing epoxy soybean oil modified resin modified by amine compound as a raw material, and the amine-containing compound contains a special nitrogen element, so that the paper-based copper-clad plate has excellent flame retardant property.
The paper-based copper-clad plate prepared by using the nitrogen-containing epoxy soybean oil modified resin prepared in step S201 and the preparation method of the nitrogen-containing epoxy soybean oil modified resin prepared in the above-mentioned first to fifth embodiments is tested, and the test data is shown in the following table:
as can be seen from the table above, the paper-based copper-clad plate prepared by the invention has good peel strength, dip soldering resistance and flame retardance, and good heat-conducting property.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention, and any modifications, equivalents and the like that are within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (2)
1. The preparation method of the nitrogen-containing epoxy soybean oil modified resin is characterized by comprising the following steps:
step S101: adding epoxidized soybean oil subjected to epoxy ring opening, bisphenol A and cardanol into a reaction kettle for addition reaction;
step S102: under an alkaline condition, adding melamine, formaldehyde and phenol into a reaction kettle for polycondensation, wherein the mass ratio of the melamine to the sum of the mass of the melamine, epoxy soybean oil subjected to epoxy ring opening, bisphenol A, cardanol, formaldehyde and phenol is 3%; and
step S103: adding a gelatinizing agent into a reaction kettle, gelatinizing for 7 minutes at 180 ℃, and then performing vacuum dehydration to prepare the nitrogen-containing epoxy soybean oil modified resin;
in step S102, the alkaline conditions are: sodium hydroxide solution at pH 7.8.
2. A method for preparing a paper-based copper-clad plate by adopting nitrogen-containing epoxy soybean oil modified resin is characterized by comprising the following steps:
step S201: dissolving nitrogen-containing epoxy soybean oil modified resin and epoxy resin in a solvent, and fully stirring to generate a mixed solution, wherein the nitrogen-containing epoxy soybean oil modified resin is prepared by the preparation method of the nitrogen-containing epoxy soybean oil modified resin according to claim 1;
step S202: curing the mixed solution to generate a resin glue solution;
step S203: coating the resin glue solution on two sides of the wood pulp paper, baking to remove the solvent, and then dip-coating the resin glue solution on two sides to obtain a sizing sheet;
step S204: superposing a plurality of sizing material sheets and a sizing foil together, putting the mixture between two steel plates, and carrying out hot pressing and cooling to prepare the nitrogenous epoxy soybean oil modified resin to prepare the paper-based copper-clad plate; the solvent comprises methanol.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591418A (en) * | 2009-02-25 | 2009-12-02 | 福建利豪电子科技股份有限公司 | A kind of preparation method of modified phenolic resins |
| CN107488331A (en) * | 2017-08-17 | 2017-12-19 | 建滔（佛冈）积层纸板有限公司 | Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613906B (en) * | 2013-11-22 | 2015-07-15 | 江苏星源航天材料股份有限公司 | Flame-resistant melamine-paraformaldehyde modified tung oil resin for copper-clad plate |
| CN111572129B (en) * | 2020-05-26 | 2021-01-08 | 北京福润达化工有限责任公司 | Preparation method of melamine modified epoxy resin glass cloth laminated board |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591418A (en) * | 2009-02-25 | 2009-12-02 | 福建利豪电子科技股份有限公司 | A kind of preparation method of modified phenolic resins |
| CN107488331A (en) * | 2017-08-17 | 2017-12-19 | 建滔（佛冈）积层纸板有限公司 | Epoxidized soybean oil modified alkyd resin glue liquid and preparation method thereof for paper-based copper-coated board |
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