TW201938630A - Method for applying reactive polymer phenol-formaldehyde resin in which a bakelite powder is mixed with a phenol-formaldehyde resin precursor - Google Patents
Method for applying reactive polymer phenol-formaldehyde resin in which a bakelite powder is mixed with a phenol-formaldehyde resin precursor Download PDFInfo
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
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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
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
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- 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
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/55—Boron-containing compounds
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- 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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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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
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2361/14—Modified phenol-aldehyde condensates
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
- Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
Description
本發明是有關於一種酚醛樹脂的應用方法,特別是指一種反應型高分子酚醛樹脂的應用方法。The invention relates to a method for applying a phenolic resin, in particular to a method for applying a reactive polymer phenolic resin.
現有普遍使用的電木(bakelite)是一種酚醛樹脂製品,主要是透過酚醛樹脂膠合纖維(紙、織物或玻璃)等支撐材料,再經過加熱加壓而製得,具備良好的電氣、機械及加工性質(如:絕緣、耐磨、耐高溫、耐燃),廣泛用於電器或交通工具的絕緣部件。Bakelite is a phenolic resin product that is commonly used. It is mainly made by supporting materials such as phenolic resin fiber (paper, fabric or glass), and then heated and pressurized. It has good electrical, mechanical and processing properties. Properties (such as: insulation, abrasion resistance, high temperature resistance, flame resistance), widely used in electrical or vehicle insulation parts.
然而,電木製品的回收處理過程容易對於環境產生負擔(如:排放二氧化碳)。However, the recycling process of bakelite products is likely to cause a burden on the environment (such as carbon dioxide emissions).
因此,本發明之目的,即在提供一種反應型高分子酚醛樹脂的應用方法,可以克服上述先前技術的缺點。Therefore, the object of the present invention is to provide a method for applying a reactive polymer phenolic resin, which can overcome the disadvantages of the foregoing prior art.
於是,本發明反應型高分子酚醛樹脂的應用方法,包含:混合一電木細粉與一酚醛樹脂前驅物,並使該電木細粉與該酚醛樹脂前驅物進行縮合反應。Therefore, the application method of the reactive polymer phenolic resin of the present invention includes: mixing a bakelite fine powder with a phenolic resin precursor, and performing a condensation reaction between the bakelite fine powder and the phenolic resin precursor.
本發明之功效在於:本發明反應型高分子酚醛樹脂的應用方法能有效回收利用電木製品再製成新的電木製品,且可提高電木製品的物性。The effect of the present invention is that the application method of the reactive polymer phenolic resin of the present invention can effectively recycle and use bakelite products to make new bakelite products, and can improve the physical properties of bakelite products.
以下將就本發明內容進行詳細說明:The following will describe the content of the present invention in detail:
由於電木製品的苯環結構上含有尚可供進行取代反應的空缺位置,即其苯酚結構上含有尚可供進行取代反應的鄰位氫/對位氫,因此可參與縮合反應形成新的電木製品。Because the benzene ring structure of bakelite products contains vacant positions that are still available for substitution reactions, that is, its phenol structure contains ortho- / para-hydrogen that is still available for substitution reactions, it can participate in the condensation reaction to form new bakelite products. .
較佳地,該酚醛樹脂前驅物是甲醛與苯酚在鹼催化下進行加成反應及縮合反應得到的預聚物。更佳地,該鹼可選自於含有氫氧化鈉、氫氧化鉀、氫氧化鋇、乙二胺、三乙胺或二甲基乙醇胺的催化劑。在本發明的具體實施例中,該鹼為氫氧化鈉水溶液。Preferably, the phenolic resin precursor is a prepolymer obtained by the addition reaction and condensation reaction of formaldehyde and phenol under alkali catalysis. More preferably, the base may be selected from catalysts containing sodium hydroxide, potassium hydroxide, barium hydroxide, ethylenediamine, triethylamine, or dimethylethanolamine. In a specific embodiment of the present invention, the base is an aqueous sodium hydroxide solution.
更佳地,該反應型高分子酚醛樹脂的應用方法,還包含:將一補強物含浸於一含有該電木細粉與該酚醛樹脂前驅物的混合物中,以得到一膠片,並熱壓該膠片以使該電木細粉與該酚醛樹脂前驅物進行縮合反應。More preferably, the application method of the reactive polymer phenolic resin further comprises: impregnating a reinforcing substance in a mixture containing the bakelite fine powder and the phenolic resin precursor to obtain a film, and hot-pressing the film. The film is subjected to a condensation reaction between the bakelite fine powder and the phenolic resin precursor.
較佳地,該電木細粉的粒徑為50 μm以下。Preferably, the particle size of the bakelite fine powder is 50 μm or less.
較佳地,該甲醛與苯酚的用量莫耳比例範圍為0.7:1~2.5:1。Preferably, the molar ratio of the amount of formaldehyde to phenol ranges from 0.7: 1 to 2.5: 1.
較佳地,該電木細粉的用量比例範圍為5~100 phr。Preferably, the dosage ratio of the bakelite fine powder ranges from 5 to 100 phr.
更佳地,該混合物還含有一有機溶劑,以調整固含量及黏度。在本發明的具體實施例中,該有機溶劑為甲醇。More preferably, the mixture also contains an organic solvent to adjust the solid content and viscosity. In a specific embodiment of the present invention, the organic solvent is methanol.
更佳地,該混合物還含有一改質劑,該改質劑是選自於經烷氧基取代的矽烷或硼酸衍生物。More preferably, the mixture also contains a modifier, the modifier being selected from alkoxy-substituted silanes or boric acid derivatives.
在本發明的具體實施例中,該經烷氧基取代的矽烷是甲基三甲氧基矽烷(methyl trimethoxysilane)。更佳地,該經烷氧基取代的矽烷的用量比例範圍為1~30 phr。In a specific embodiment of the present invention, the alkoxy-substituted silane is methyl trimethoxysilane. More preferably, the proportion of the alkoxy-substituted silane used ranges from 1 to 30 phr.
該硼酸衍生物可為硼酸[boric acid, B(OH)3 ]、經烴基取代的硼酸[boronic acid, R-B(OH)2 及borinic acid, RR'-B(OH)]。在本發明的具體實施例中,該硼酸衍生物為硼酸。更佳地,該硼酸衍生物的用量比例範圍為1~20 phr。The boric acid derivative can be boric acid [boric acid, B (OH) 3 ], hydrocarbyl-substituted boric acid [boronic acid, RB (OH) 2 and borinic acid, RR'-B (OH)]. In a specific embodiment of the present invention, the boric acid derivative is boric acid. More preferably, the usage ratio of the boric acid derivative ranges from 1 to 20 phr.
更佳地,該補強物是選自於一紙片或一布片。在本發明的具體實施例中,該補強物是一捲筒紙。More preferably, the reinforcement is selected from a piece of paper or a piece of cloth. In a specific embodiment of the invention, the reinforcement is a roll of paper.
在本發明的具體實施例中,該熱壓的溫度約為150~180℃。In a specific embodiment of the present invention, the temperature of the hot pressing is about 150-180 ° C.
本發明將就以下實施例來作進一步說明,但應瞭解的是,該等實施例僅為例示說明之用,而不應被解釋為本發明實施之限制。The present invention will be further described with reference to the following examples, but it should be understood that these examples are for illustrative purposes only and should not be construed as limiting the implementation of the present invention.
[[ 實施例Examples 1]1]
將53 g聚甲醛(paraformaldehyde)溶於60 g水中,加入94 g苯酚混合均勻,加入3 g 40 wt%氫氧化鈉水溶液調整pH值至8.5-9.0以催化加成反應及縮合反應進行,並在攪拌下加熱至回流(100℃)約2 h,以得到一預聚物。Dissolve 53 g of paraformaldehyde in 60 g of water, add 94 g of phenol and mix well. Add 3 g of 40 wt% sodium hydroxide aqueous solution to adjust the pH to 8.5-9.0 to catalyze the addition reaction and condensation reaction. Heat to reflux (100 ° C) for about 2 h with stirring to obtain a prepolymer.
在該預聚物中加入5 phr且粒徑為50 μm(約300 mesh)以下的電木細粉(作為反應型高分子,其是將電木製品回收後粉碎研磨而得),再加入90 g甲醇,以調整固含量達50%及調整黏度。Add 5 phr of bakelite fine powder with a particle size of 50 μm (about 300 mesh) or less (as a reactive polymer, which is obtained by crushing and grinding bakelite products), and then add 90 g Methanol to adjust the solid content to 50% and adjust the viscosity.
將一捲筒紙連續含浸於上述含有該電木細粉與該預聚物的甲醇溶液中,抽真空並進行濃縮以脫除水及苯酚,接著在120℃烘箱中以30 m/min的速度連續進行縮合反應,乾燥後裁切成半固化的膠片。A roll of paper was continuously immersed in the above methanol solution containing the bakelite fine powder and the prepolymer, vacuumed and concentrated to remove water and phenol, and then in a 120 ° C oven at a speed of 30 m / min The condensation reaction is continuously performed, and after drying, it is cut into a semi-cured film.
隨後將5張上述膠片平放在兩片光滑的不鏽鋼板之間,從上下施加700 mmHg的壓力並加熱至150~180℃維持30 min以進行縮合反應,最後得到厚度約為0.5~0.7 mm的電木板E1。另外,可依所需的電木板厚度改變膠片數量。Subsequently, 5 sheets of the above-mentioned film were laid flat between two smooth stainless steel plates, and a pressure of 700 mmHg was applied from above and below and heated to 150-180 ° C for 30 minutes to perform a condensation reaction, and finally a thickness of about 0.5-0.7 mm was obtained. Bakelite E1. In addition, the number of films can be changed according to the required thickness of the bakelite.
[[ 實施例Examples 2~5]2 ~ 5]
實施例2~5的製造方法與實施例1類似,差異之處在於將該電木細粉的添加量分別改變為10、20、30、50 phr,分別得到實施例2~5的電木板E2~E5。The manufacturing method of Examples 2 to 5 is similar to that of Example 1, except that the addition amount of the bakelite fine powder is changed to 10, 20, 30, 50 phr, respectively, and the bakelite E2 of examples 2 to 5 are obtained. ~ E5.
[[ 實施例Examples 6]6]
實施例6的製造方法與實施例1類似,差異之處在於在該預聚物中另外加入20 phr甲基三甲氧基矽烷,得到實施例6的電木板E6。The manufacturing method of Example 6 is similar to that of Example 1, except that 20 phr of methyltrimethoxysilane is added to the prepolymer to obtain the bakelite E6 of Example 6.
[[ 實施例Examples 7]7]
實施例7的製造方法與實施例1類似,差異之處在於在該預聚物中另外加入10 phr硼酸,得到實施例7的電木板E7。The manufacturing method of Example 7 is similar to that of Example 1, except that 10 phr of boric acid is added to the prepolymer to obtain the bakelite E7 of Example 7.
[[ 實施例Examples 8]8]
實施例8的製造方法與實施例1類似,差異之處在於在該預聚物中另外加入20 phr甲基三甲氧基矽烷,並將該電木細粉的添加量改變為60 phr,得到實施例8的電木板E8。The manufacturing method of Example 8 is similar to that of Example 1, except that 20 phr of methyltrimethoxysilane is added to the prepolymer, and the addition amount of the bakelite fine powder is changed to 60 phr. Bakelite E8 of Example 8.
[[ 實施例Examples 9]9]
實施例9的製造方法與實施例1類似,差異之處在於在該預聚物中另外加入20 phr甲基三甲氧基矽烷及10 phr硼酸,並將該電木細粉的添加量改變為60 phr,得到實施例9的電木板E9。The manufacturing method of Example 9 is similar to that of Example 1, except that 20 phr of methyltrimethoxysilane and 10 phr of boric acid are added to the prepolymer, and the amount of the bakelite fine powder is changed to 60. phr to obtain the bakelite E9 of Example 9.
[[ 比較例]Comparative Example]
比較例的製造方法與實施例1類似,差異之處在於在該預聚物中不加入該電木細粉,最後得到比較例的電木板CE。The manufacturing method of the comparative example is similar to that of Example 1, except that the bakelite fine powder is not added to the prepolymer, and finally the bakelite CE of the comparative example is obtained.
[[ 電木板性質測試Bakelite property test ]]
分別測量上述實施例1~9及比較例的電木板E1~E9及CE的蕭氏硬度(Shore D)、彎曲強度及軟化溫度(Tmax
),結果分別如下表1所示。 【表1】
綜上所述,本發明反應型高分子酚醛樹脂的應用方法藉由添加電木細粉作為反應型高分子,有效回收利用電木製品再製成新的電木製品(電木板),不僅可降低回收處理的困擾及對於環境的負擔,還可以提高電木製品的硬度及熱安定性等性質,並節省製程所需的原物料,故確實能達成本發明之目的。In summary, the application method of the reactive high-molecular phenolic resin of the present invention, by adding bakelite fine powder as a reactive polymer, effectively recycles bakelite products and then makes new bakelite products (bakelite), which can not only reduce recycling. The trouble of treatment and the burden on the environment can also improve the hardness and thermal stability of bakelite products, and save the raw materials required for the process, so it can indeed achieve the purpose of cost invention.
惟以上所述者,僅為本發明之實施例而已,當不能以此限定本發明實施之範圍,凡是依本發明申請專利範圍及專利說明書內容所作之簡單的等效變化與修飾,皆仍屬本發明專利涵蓋之範圍內。However, the above are only examples of the present invention. When the scope of implementation of the present invention cannot be limited in this way, any simple equivalent changes and modifications made in accordance with the scope of the patent application and the content of the patent specification of the present invention are still Within the scope of the invention patent.
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TW107107907A TWI647251B (en) | 2018-03-08 | 2018-03-08 | Application method of reactive polymer phenolic resin |
CN201810890085.3A CN110240724A (en) | 2018-03-08 | 2018-08-07 | The application method of reactive polymer phenolic resin |
KR1020180136461A KR20200068036A (en) | 2018-03-08 | 2018-11-08 | Method for reprocessing recycled phenol formaldehyde resin powders |
JP2018230005A JP2019157111A (en) | 2018-03-08 | 2018-12-07 | Method of using phenol-formaldehyde resin product |
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CN103265674B (en) * | 2013-05-11 | 2015-05-13 | 北京化工大学 | Phenol-polyaldehyde prepolymer modified environment-friendly phenolic resin and preparation method thereof |
CN104151556A (en) * | 2013-05-13 | 2014-11-19 | 北京化工大学 | Preparation of polyborosiloxane and phenolic resin heat resistant modification method |
CN104448694A (en) * | 2014-12-10 | 2015-03-25 | 广东品翔环保科技有限公司 | Process for recycling, regenerating and molding waste phenolic resin composite materials |
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2018
- 2018-03-08 TW TW107107907A patent/TWI647251B/en not_active IP Right Cessation
- 2018-08-07 CN CN201810890085.3A patent/CN110240724A/en active Pending
- 2018-11-08 KR KR1020180136461A patent/KR20200068036A/en unknown
- 2018-12-07 JP JP2018230005A patent/JP2019157111A/en active Pending
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CN110240724A (en) | 2019-09-17 |
KR20200068036A (en) | 2020-06-15 |
TWI647251B (en) | 2019-01-11 |
JP2019157111A (en) | 2019-09-19 |
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