Preparation method of high-temperature-resistant engineering plastic amino-terminated polyarylene ether nitrile toughened BT resin
By synthesizing amino-terminated polyarylethernitrile and bismaleimide for Michael addition reaction and blending with cyanate ester, a high-temperature-resistant amino-terminated polyarylethernitrile toughened BT resin was prepared, which solved the problems of insufficient toughness and reduced heat resistance of BT resin, achieved high strength, high toughness, and high heat resistance, and expanded its application potential in the field of microelectronics.
Patent Information
- Application Number
- CN202510182511.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-19
- Publication Date
- 2025-05-27
AI Technical Summary
The existing BT resin has poor toughness and sacrifices heat resistance while toughening, which limits its wide application in the field of microelectronics.
By synthesizing amino-terminated polyarylethernitrile and undergoing Michael addition reaction with bismaleimide to extend the chain toughening, then blending with cyanate ester, and using a small amount of amino-containing phthalene as a curing agent, high temperature-resistant amino-terminated polyarylethernitrile toughening BT resin was prepared by grading temperature control treatment.
It not only enhances the toughness of BT resin, but also further consolidates its heat resistance, providing a new preparation method, suitable for the production of high-strength, high-strength, high-heat resistance BT resin, with broader application prospects.
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Figure CN120040750A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of polymer materials, and specifically relates to a preparation method of an amino-terminated polyarylether nitrile toughened BT resin, a high-temperature resistant engineering plastic. Background Art
[0002] As a kind of high-performance thermosetting polymer, bismaleimide-triazine (BT) resin has been widely used in microelectronics fields such as printed circuit boards and semiconductor packaging due to its high heat resistance, low water absorption, excellent mechanical properties and insulation properties. However, at present, due to the three-dimensional network with high crosslinking degree, the toughness of BT resin is poor, which imposes certain limitations on the application of BT resin. Using thermoplastic plastics to toughen thermosetting resins is a research hotspot, but at the same time of toughening, the heat resistance of the resin will be sacrificed.
[0003] Polyarylether nitrile (PEN) is a kind of high-temperature resistant engineering plastic, which exhibits outstanding properties such as high heat resistance, creep resistance, high strength, high rigidity, high toughness and excellent electrical properties due to its special molecular structure. Such materials have extensive potential applications in fields such as aerospace, automobile manufacturing, electronic and electrical, and machining.
[0004] If BT resin can be modified to have the excellent properties of polyarylether nitrile while being toughened, it will enable BT resin to be more widely used. Summary of the Invention
[0005] The purpose of the present invention is to address the above problems and provide a preparation method of an amino-terminated polyarylether nitrile toughened BT resin, a high-temperature resistant engineering plastic. The present invention first synthesizes an amino-terminated polyarylether nitrile, then conducts a Michael addition reaction with bismaleimide for chain extension and toughening, and finally blends it with cyanate ester, and uses a small amount of amino-containing phthalonitrile as a curing agent, and through hierarchical temperature control treatment, a high-temperature resistant amino-terminated polyarylether nitrile toughened BT resin is prepared.
[0006] The high-temperature resistant amino-terminated polyarylether nitrile toughened BT resin provided by the present invention can not only toughen and strengthen BT resin, but also further consolidate the heat resistance of BT resin, thereby providing a new preparation method for producing high-strength, high-toughness and high-heat-resistant BT resin, and having a broader application prospect in the field of electronic materials.
[0007] In order to achieve the above purpose, the technical solution provided by the present invention is as follows:
[0008] A preparation method of an amino-terminated polyarylether nitrile toughened BT resin, a high-temperature resistant engineering plastic, specifically includes the following steps:
[0009] (1) Synthesis of amino-terminated polyarylether nitrile
[0010] Polyarylether nitrile was synthesized by nucleophilic substitution reaction to obtain amino-terminated polyarylether nitrile;
[0011] (2) Modification of bismaleimide with amino-terminated polyarylether nitrile
[0012] At a certain temperature and time, amino-terminated polyarylether nitrile and bismaleimide were subjected to Michael addition reaction in a solvent in a certain ratio for chain extension modification to obtain amino-terminated polyarylether nitrile modified bismaleimide;
[0013] (3) Amino-terminated polyarylether nitrile modified bismaleimide
[0014] Phthalonitrile was used as a curing agent, and cyanate ester and polyarylether nitrile modified bismaleimide were blended in a solvent in a certain ratio at a certain time and temperature to obtain a blend. Through hierarchical temperature control, amino-terminated polyarylether nitrile modified BT resin was prepared, and its structural formula is as follows:
[0015]
[0016] Furthermore, in step (1), the synthesis of the amino-terminated polyarylether nitrile is as follows: 2,6-dichlorobenzonitrile and bisphenol A in a set ratio were added as reactants into a three-necked flask equipped with a mechanical stirrer, a water separator, and a thermometer, and potassium carbonate was added as a catalyst to obtain a mixture powder; 15 mL of toluene and 15 mL of water were injected into the water separator; the mixture powder was added into a mixed solvent of N-methylpyrrolidone and toluene; among them, (1-1.5) mL of the mixed solvent was added per 1 g of the mixture powder, and in the mixed solvent, the volume ratio of N-methylpyrrolidone to toluene was 3:1; the obtained mixed solution was heated to 145-150 °C in an electric heating mantle and kept at a constant temperature of 145-150 °C for 2 h; after dehydration, the temperature was raised to 190-200 °C, and p-aminophenol dehydrated with potassium carbonate was added at 190-200 °C and reacted at a constant temperature for 100-120 min; finally, the temperature was lowered to 150 °C, and the obtained reaction solution was poured into a 0.2 mol / L hydrochloric acid solution and stirred to obtain a strip-shaped solid; the obtained strip-shaped solid A was soaked in a 0.2 mol / L hydrochloric acid solution for 12 h, crushed, and then washed 3-5 times until the solution was neutral; the washed powder was placed in a vacuum oven and dried for 12 h to obtain the amino-terminated polyarylether nitrile, and the synthesis steps are as follows:
[0017]
[0018] Further, in step (2), the bismaleimide is mainly diphenylmethane bismaleimide (a), N,N'-m-phenylene bismaleimide (b), N,N'-(1,4-phenylene) bismaleimide (c), 1,2-bis(maleimide)ethane (d), N,N'-tetramethylene bismaleimide (e), and their structures are as follows:
[0019]
[0020] R1 is any structure among a - e.
[0021] Further, in step (2), the molar ratio of the amino-terminated polyarylether nitrile to the bismaleimide is 2 - 4:1; the temperature of the Michael addition reaction is 50 - 120 °C (specifically, it can be 50 °C, 60 °C, 70 °C, 80 °C, 90 °C, 100 °C, 110 °C, 120 °C, etc.), and the time is 1 - 6 h (specifically, it can be 1 h, 2 h, 3 h, 4 h, 5 h, 6 h, etc.).
[0022] Further, the solvent described in step (2) is N,N-dimethylformamide, N,N-dimethylacetamide, or N-methyl-2-pyrrolidone.
[0023] Further, in step (3), the types of cyanate esters are mainly bisphenol A cyanate ester (f), phenol AF cyanate ester (g), bisphenol E cyanate ester (h), tetramethyl bisphenol F cyanate ester (i), and their structures are as follows:
[0024]
[0025] R2 is any structure among f - i.
[0026] Further, in step (3), the types of phthalonitrile are mainly 3-APN, 4-APN, 4-aminophthalonitrile, and their structures are as follows:
[0027]
[0028] Further, in step (3), the blending temperature and time are 100 - 150 °C and 1 - 8 hours respectively, and the blending solvent is mainly N,N-dimethylformamide, N,N-dimethylacetamide, or N-methyl-2-pyrrolidone.
[0029] Further, in step (3), the mass ratio of the amino-terminated polyarylether nitrile modified bismaleimide to the cyanate ester is 10-90:90-10; the mass ratio of phthalonitrile to the BT resin is 1-10% (specifically, it can be 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, etc.), and the solid content is 30-70% (specifically, it can be 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, etc.).
[0030] Further, in step (3), when the amino-terminated polyarylether nitrile modifies the BT resin, the mixture is cast into a preheated mold, degassed under vacuum at 120°C, and subjected to a stepwise temperature control treatment at 140-210°C. After the heat treatment, it is naturally cooled to room temperature, and the amino-terminated polyarylether nitrile modified BT resin is obtained after demolding.
[0031] Compared with the existing technologies, the beneficial effects of the present invention are as follows:
[0032] (1) By synthesizing amino-terminated polyarylether nitriles with different molecular weights and performing Michael addition reaction with bismaleimide, the toughness of the BT resin is regulated.
[0033] (2) By introducing a small amount of phthalonitrile as a curing agent, the compatibility between the polyarylether nitrile and the BT resin is improved, and the heat resistance of the BT resin is increased. Description of the Drawings
[0034] Figure 1 The DMA curve of the BT resin toughened with amino-terminated polyarylether nitriles with different molecular weights.
[0035] Figure 2 The gelation time of the BT resin toughened with amino-terminated polyarylether nitriles with different molecular weights.
[0036] Figure 3 The impact strength of the composites of the BT resin toughened with amino-terminated polyarylether nitriles with different molecular weights.
[0037] Figure 4 The flexural strength of the composites of the BT resin toughened with amino-terminated polyarylether nitriles with different molecular weights. Detailed Embodiments
[0038] All features disclosed in this specification, or all steps in the disclosed methods or processes, except for mutually exclusive features and / or steps, can be combined in any manner.
[0039] Any feature disclosed in this specification (including the claims and abstract), unless specifically stated, can be replaced by other equivalent or features with similar purposes. That is, unless specifically stated, each feature is only an example of a series of equivalent or similar features.
[0040] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the embodiments and the accompanying drawings of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.
[0041] Embodiment 1:
[0042] A preparation method of a high-temperature resistant engineering plastic amino-terminated polyarylether nitrile toughened BT resin specifically includes the following steps:
[0043] Step 1 Synthesis of amino-terminated polyarylether nitrile
[0044] 1.1 Add 2,6-dichlorobenzonitrile and bisphenol A as reactants in a three-necked flask equipped with a mechanical stirrer, a water separator, and a thermometer, with a mass ratio of 2:4, and add potassium carbonate as a catalyst to obtain a mixture powder; 1.2 Add the mixture powder obtained in step 1.1 to a mixed solvent of N-methylpyrrolidone and toluene to obtain a mixed solution A; wherein, 1.3 mL of the mixed solvent is added per 1 g of the mixture powder, and in the mixed solvent, the volume ratio of N-methylpyrrolidone to toluene is 3:1;
[0045] 1.3 The mixed solution A obtained in step 1.2 is heated to 146 °C in an electric heating mantle and kept at a constant temperature of 146 °C for 2 h; after dehydration, the temperature is raised to 195 °C, and p-aminophenol dehydrated with potassium carbonate is added at 195 °C and kept at a constant temperature for 110 min; finally, the temperature is lowered to 150 °C, and the obtained reaction solution is poured into a 0.2 mol / L hydrochloric acid solution, stirred, and strip-shaped solid A is obtained;
[0046] 1.4 The strip-shaped solid A obtained in step 1.3 is soaked in a 0.2 mol / L hydrochloric acid solution for 12 h, crushed, and then washed 4 times until the solution is neutral; the washed powder is placed in a vacuum oven and dried for 12 h to obtain the amino-terminated polyarylether nitrile.
[0047] Step 2 Preparation of amino-terminated polyarylether nitrile modified bismaleimide
[0048] React the amino-terminated polyarylether nitrile and diphenylmethane bismaleimide at a molar ratio of 2:1 at 90 °C for 4 hours, using N,N-dimethylformamide as a solvent and a solid content of 40 wt%, to obtain the amino-terminated polyarylether nitrile modified bismaleimide.
[0049] Step 3 Preparation of amino-terminated polyarylether nitrile modified BT resin
[0050] The amino - terminated polyarylether nitrile - modified bismaleimide and bisphenol A - type cyanate ester were blended in N,N - dimethylformamide at a mass ratio of 7:3. The blending temperature and time were 120 °C and 2 h respectively to obtain a blended solution. The mixture was cast into a pre - heated mold, degassed under vacuum at 120 °C, and the curing procedure was 1 h at 160 °C and 180 °C respectively, and 2 h at 220 °C and 240 °C respectively. After the heat treatment, it was naturally cooled to room temperature, and after demolding, the amino - terminated polyarylether nitrile - modified BT resin was obtained and named PEN - 1.
[0051] Example 2:
[0052] A preparation method of a high - temperature - resistant engineering plastic, amino - terminated polyarylether nitrile - toughened BT resin, specifically includes the following steps:
[0053] Step 1: Synthesis of amino - terminated polyarylether nitrile
[0054] 1.1 Add 2,6 - dichlorobenzonitrile and bisphenol A as reactants in a three - necked flask equipped with a mechanical stirrer, a water separator, and a thermometer at a mass ratio of 3:4, and add potassium carbonate as a catalyst to obtain a mixture powder; 1.2 Add the mixture powder obtained in step 1.1 into a mixed solvent of N - methylpyrrolidone and toluene to obtain a mixed solution A; wherein, 1 mL of the mixed solvent is added per 1 g of the mixture powder, and in the mixed solvent, the volume ratio of N - methylpyrrolidone to toluene is 3:1;
[0055] 1.3 The mixed solution A obtained in step 1.2 is heated to 145 °C in an electric heating mantle and kept at a constant temperature of 145 °C for 2 h; after dehydration, the temperature is raised to 190 °C, and p - aminophenol dehydrated with potassium carbonate is added at 190 °C and kept at a constant temperature for 100 min; finally, the temperature is lowered to 150 °C, and the obtained reaction solution is poured into a 0.2 mol / L hydrochloric acid solution and stirred to obtain a strip - shaped solid A;
[0056] 1.4 The strip - shaped solid A obtained in step 1.3 is soaked in a 0.2 mol / L hydrochloric acid solution for 12 h, crushed, and then washed 3 times until the solution is neutral; the washed powder is placed in a vacuum oven and dried for 12 h to obtain the amino - terminated polyarylether nitrile.
[0057] Step 2: Preparation of amino - terminated polyarylether nitrile - modified bismaleimide
[0058] The amino - terminated polyarylether nitrile and dimethylxylene bismaleimide were reacted at a molar ratio of 2:1 at 90 °C for 4 h, using N,N - dimethylformamide as a solvent and with a solid content of 40 wt%, to obtain the amino - terminated polyarylether nitrile - modified bismaleimide.
[0059] Step 3: Preparation of amino - terminated polyarylether nitrile - modified BT resin
[0060] The amino - terminated polyarylether nitrile modified bismaleimide and bisphenol A type cyanate ester were blended in N, N - dimethylformamide at a mass ratio of 7:3. The blending temperature and time were 120 °C and 2 h respectively to obtain a blended solution. The mixture was cast into a preheated mold, degassed under vacuum at 120 °C, and the curing procedure was 1 hour at 160 °C and 180 °C respectively, and 2 hours at 220 °C and 240 °C respectively. After the heat treatment, it was naturally cooled to room temperature, and after demolding, the amino - terminated polyarylether nitrile modified BT resin was obtained, named PEN - 2.
[0061] Example 3:
[0062] A preparation method of a high - temperature resistant engineering plastic, amino - terminated polyarylether nitrile toughened BT resin, specifically includes the following steps:
[0063] Step 1: Synthesis of amino - terminated polyarylether nitrile
[0064] 1.1 2,6 - dichlorobenzonitrile and bisphenol A were added as reactants in a three - necked flask equipped with a mechanical stirrer, a water separator, and a thermometer at a mass ratio of 7:8, and potassium carbonate was added as a catalyst to obtain a mixture powder; 1.2 The mixture powder obtained in step 1.1 was added to a mixed solvent of N - methylpyrrolidone and toluene to obtain a mixed solution A; wherein, 1.2 mL of the mixed solvent was added per 1 g of the mixture powder, and in the mixed solvent, the volume ratio of N - methylpyrrolidone to toluene was 3:1;
[0065] 1.3 The mixed solution A obtained in step 1.2 was heated to 146 °C in an electric heating mantle and reacted at a constant temperature of 146 °C for 2 h; after dehydration, the temperature was raised to 193 °C, and p - aminophenol dehydrated with potassium carbonate was added at 193 °C and reacted at a constant temperature for 110 min; finally, the temperature was lowered to 150 °C, and the obtained reaction solution was poured into a 0.2 mol / L hydrochloric acid solution and stirred to obtain a strip - shaped solid A;
[0066] 1.4 The strip - shaped solid A obtained in step 1.3 was soaked in a 0.2 mol / L hydrochloric acid solution for 12 h, then crushed, and washed 3 - 5 times until the solution was neutral; the washed powder was placed in a vacuum oven and dried for 12 h to obtain the amino - terminated polyarylether nitrile.
[0067] Step 2: Preparation of amino - terminated polyarylether nitrile modified bismaleimide
[0068] The amino - terminated polyarylether nitrile and dimethylbenzene methane bismaleimide were reacted at a molar ratio of 2:1 at 90 °C for 4 h, using N, N - dimethylformamide as a solvent and the solid content was 40 wt%, to obtain the amino - terminated polyarylether nitrile modified bismaleimide.
[0069] Step 3: Preparation of amino - terminated polyarylether nitrile modified BT resin
[0070] The amino-terminated polyarylether nitrile modified bismaleimide and bisphenol A cyanate ester were blended in N,N-dimethylformamide at a mass ratio of 7:3. The blending temperature and time were 120 °C and 2 h respectively to obtain a blended solution. The mixture was cast into a preheated mold, degassed under vacuum at 120 °C, and the curing procedure was 1 h at 160 and 180 °C, and 2 h at 220 and 240 °C respectively. After the heat treatment, it was naturally cooled to room temperature, and after demolding, the amino-terminated polyarylether nitrile modified BT resin was obtained and named PEN-3.
[0071] Example 4:
[0072] Step 1: Synthesis of amino-terminated polyarylether nitrile
[0073] 1.1 2,6-Dichlorobenzonitrile and bisphenol A were added as reactants in a three-necked flask equipped with a mechanical stirrer, a water separator, and a thermometer at a mass ratio of 11:12, and potassium carbonate was added as a catalyst to obtain a mixture powder; 1.2 The mixture powder obtained in step 1.1 was added to a mixed solvent of N-methylpyrrolidone and toluene to obtain a mixed solution A; wherein, 1.35 mL of the mixed solvent was added per 1 g of the mixture powder, and in the mixed solvent, the volume ratio of N-methylpyrrolidone to toluene was 3:1;
[0074] 1.3 The mixed solution A obtained in step 1.2 was heated to 147 °C in an electric heating mantle and reacted at a constant temperature of 147 °C for 2 h; after dehydration, the temperature was raised to 196 °C, and p-aminophenol dehydrated with potassium carbonate was added at 196 °C and reacted at a constant temperature for 108 min; finally, the temperature was lowered to 150 °C, and the obtained reaction solution was poured into a 0.2 mol / L hydrochloric acid solution and stirred to obtain a strip-shaped solid A;
[0075] 1.4 The strip-shaped solid A obtained in step 1.3 was soaked in a 0.2 mol / L hydrochloric acid solution for 12 h, crushed, and then washed 3 times until the solution was neutral; the washed powder was placed in a vacuum oven and dried for 12 h to obtain the amino-terminated polyarylether nitrile.
[0076] Step 2: Preparation of amino-terminated polyarylether nitrile modified bismaleimide
[0077] The amino-terminated polyarylether nitrile and dimethylbenzene methane bismaleimide were reacted at a molar ratio of 2:1 at 90 °C for 4 h, using N,N-dimethylformamide as a solvent and a solid content of 40 wt%, to obtain the amino-terminated polyarylether nitrile modified bismaleimide.
[0078] Step 3: Preparation of amino-terminated polyarylether nitrile modified BT resin
[0079] The amino-terminated polyarylether nitrile modified bismaleimide and bisphenol A cyanate ester were blended in N,N-dimethylformamide at a mass ratio of 7:3. The blending temperature and time were 120 °C and 2 h respectively to obtain a blended solution. The mixture was cast into a preheated mold, and the air bubbles were removed under vacuum at 120 °C. The curing procedure was 1 h at 160 °C and 180 °C respectively, and 2 h at 220 °C and 240 °C respectively. After the heat treatment was completed, it was naturally cooled to room temperature. After demolding, the amino-terminated polyarylether nitrile modified BT resin was obtained and named PEN-4.
[0080] Comparative Example 1
[0081] 70 parts of dimethylbenzene methane bismaleimide and 30 parts of bisphenol A cyanate ester were added to N,N-dimethylacetamide solvent to prepare a 30% mixture, and ultrasonic treatment was carried out for 1 h. Subsequently, it was placed in a vacuum oven at 120 °C to remove the solvent for 1 h, and then placed in a programmed temperature rise equipment for stepwise temperature control treatment. The heat treatment temperatures were 1 h at 160 °C, and 2 h at 180 °C, 220 °C and 240 °C respectively to prepare BT resin.
[0082] The resins obtained in Examples 1-4 and Comparative Example 1 were subjected to performance tests, as shown specifically in Figures 1-4 , Figure 1 which are the DMA curves of BT resins toughened by amino-terminated polyarylether nitriles with different molecular weights. As can be seen from Figure 1 , the glass transition temperatures of BT resin, PEN-1, PEN-2, PEN-3 and PEN-4 are 247 °C, 260 °C, 287 °C, 281 °C and 259 °C respectively. Figure 2 is the gelation time of BT resins toughened by amino-terminated polyarylether nitriles with different molecular weights. Figure 3 is the impact strength of composites of BT resins toughened by amino-terminated polyarylether nitriles with different molecular weights. As can be seen from Figure 3 , the impact strengths of BT resin, PEN-1, PEN-2, PEN-3 and PEN-4 are 65 kJ / m 2 , 92 kJ / m 2 , 122 kJ / m 2 , 135 kJ / m 2 and 87 kJ / m 2 respectively. High impact strength represents high toughness of the resin. Figure 4 is the flexural strength of composites of BT resins toughened by amino-terminated polyarylether nitriles with different molecular weights. As can be seen from Figure 4 , the flexural strengths of BT resin, PEN-1, PEN-2, PEN-3 and PEN-4 are 580 MPa, 620 MPa, 687 MPa, 510 MPa and 490 MPa respectively.
[0083] The above-described embodiments merely represent the specific implementation manners of the present application. The description thereof is relatively specific and detailed, but it should not be construed as a limitation to the protection scope of the present application. It should be noted that for those of ordinary skill in the art, without departing from the concept of the technical solution of the present application, several variations and improvements can still be made, and these all fall within the protection scope of the present application.
[0084] This background art section is provided to generally present the context of the present invention. The work of the currently named inventors, to the extent described in this background art section, and aspects of the work that are not prior art as of the filing date of this application are neither expressly nor impliedly admitted to be prior art to the present invention.
Claims
1. A method for preparing amino-terminated polyarylethernitrile toughened BT resin for high temperature resistant engineering plastics, characterized in that: The steps include: (1) synthesizing poly(arylether nitrile) by nucleophilic substitution reaction to obtain amino-terminated poly(arylether nitrile); (2) at a certain temperature and time, amino-terminated poly(arylether nitrile) and bismaleimide are subjected to Michael addition reaction in a solvent in a certain ratio to perform chain extension modification, thereby obtaining amino-terminated poly(arylether nitrile) modified bismaleimide; (3) Using phthalonitrile as a curing agent, cyanate ester and poly(arylene ether nitrile) modified bismaleimide are blended in a solvent to obtain a blend, and amino-terminated poly(arylene ether nitrile) toughened BT resin is prepared by graded temperature control.
2. The method for preparing the amino-terminated polyarylether nitrile toughened BT resin according to claim 1, characterized in that: The specific steps of synthesizing the amino-terminated poly(arylene ether nitrile) in step (1) are: In a three-necked flask equipped with a mechanical stirrer, a water separator and a thermometer, 2,6-dichlorobenzonitrile and bisphenol A with a set ratio are added as reactants, and potassium carbonate is added as a catalyst to obtain a mixture powder; toluene and water are injected into the water separator; the obtained mixture powder is added into a mixed solvent of N-methylpyrrolidone and toluene; the obtained mixed solution is heated in an electric heating jacket until a reaction occurs; after dehydration, the temperature is increased again, and p-aminophenol dehydrated with potassium carbonate is added, and the reaction is carried out at a constant temperature for a period of time; finally, the temperature is lowered, and the obtained reaction solution is poured into a hydrochloric acid solution, stirred, and a strip-shaped solid is obtained; the obtained strip-shaped solid A is soaked in a hydrochloric acid solution and then crushed, and then washed until the solution is neutral; the washed powder is placed in a vacuum oven and dried to obtain an amino-terminated polyarylethernitrile.
3. The method for preparing the amino-terminated polyarylether nitrile toughened BT resin according to claim 1, characterized in that: In step (2), the bismaleimide is diphenylmethane bismaleimide, N,N'-m-phenylene bismaleimide, N,N'-(1,4-phenylene) bismaleimide, 1,2-bis(maleimide)ethane, N,N'-tetramethylene bismaleimide; the molar ratio of amino-terminated polyarylether nitrile to bismaleimide is 2 to 4:
1.
4. The method for preparing the amino-terminated polyarylether nitrile toughened BT resin according to claim 1, characterized in that: In step (2), the temperature of the Michael addition reaction is 50 to 120° C. and the time is 1 to 6 hours.
5. The method for preparing amino-terminated polyarylether nitrile toughened BT resin according to claim 1, characterized in that: The solvents described in step (2) and step (3) are N,N-dimethylformamide, N,N-dimethylacetamide or N-methyl-2-pyrrolidone.
6. The method for preparing amino-terminated poly(arylene ether nitrile) toughened BT resin according to claim 1, characterized in that: In step (3), the cyanate ester is selected from bisphenol A cyanate ester, phenol AF cyanate ester, bisphenol F cyanate ester, bisphenol E cyanate ester, and bisphenol M cyanate ester; the phthalonitrile is selected from 3-APN, 4-APN, and 4-aminophthalonitrile; the mass ratio of the polyarylether nitrile-modified bismaleimide and the cyanate ester is 10-90:90-10; the phthalonitrile accounts for 1-10% of the mass of the BT resin, and the solid content is 30-70%.
7. The method for preparing amino-terminated polyarylethernitrile toughened BT resin according to claim 1, characterized in that: In step (3), the graded temperature control treatment is to cast the mixture into a preheated mold, remove bubbles at 120°C in vacuum, and perform graded temperature control treatment at 140-210°C. After the heat treatment, it is naturally cooled to room temperature, and the amino-terminated polyarylether nitrile modified BT resin is obtained after demolding.
8. The method for preparing the amino-terminated poly(arylene ether nitrile) toughened BT resin according to claim 2, characterized in that: In step (1), the volume ratio of toluene to water is 1:1; in the mixed solvent, the volume ratio of N-methylpyrrolidone to toluene is 3:1; the ratio of the mass g of the mixture powder to the volume mL of the mixed solvent is 1:1-1.5; the obtained mixed solution is heated to 145-150°C in an electric heating jacket, and is kept at 145-150°C for 2 hours; after dehydration, the temperature is raised to 190-200°C, and p-aminophenol dehydrated with potassium carbonate is added at 190-200°C for constant temperature reaction for 100-120 minutes; finally, the temperature is lowered to 150°C, and the obtained reaction solution is poured into a 0.2 mol / L hydrochloric acid solution, stirred to obtain a strip-shaped solid; the obtained strip-shaped solid A is soaked in a 0.2 mol / L hydrochloric acid solution for 12 hours, crushed, and then washed 3-5 times until the solution is neutral; the washed powder is placed in a vacuum oven and dried for 12 hours.
9. An amino-terminated polyarylethernitrile toughened BT resin prepared according to the method of any one of claims 1 to 8.
10. Use of the amino-terminated polyarylethernitrile toughened BT resin according to claim 9 in the field of electronic materials.