High-temperature stable mold release agent and preparation method thereof

Abstract

The invention relates to the field of semiconductor packaging, and particularly discloses a high-temperature-stable mold release agent and a preparation method thereof.The high-temperature-stable mold release agent is prepared from, by weight, 18-22 parts of blending rubber and 6-8 parts of functional reinforcing agent; 4 parts of a wear-resistant component, 4 to 5 parts of a mold cleaning agent, 0.02 to 0.04 part of a cross-linking agent and 0.0006 to 0.0012 part of a polymerization inhibitor; the functional reinforcing agent and the wear-resistant component are added into the mold release agent, and the functional reinforcing agent contains-Si-O-Si bonds, benzene rings, trifluoromethyl and unsaturated double bonds, not only can be chemically crosslinked with a blended rubber material, but also can react with the wear-resistant component, so that the heat resistance, the mechanical property, the demolding effect and the wear resistance of the mold release agent are synergistically improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of semiconductor packaging, more particularly, it relates to a high-temperature stable mold release agent and a preparation method thereof. BACKGROUND

[0002] The selection of semiconductor packaging materials and defect control are the key to ensure the final performance, reliability and cost of chips. At present, epoxy plastic packaging materials occupy an absolute mainstream due to their comprehensive advantages, and ceramic and metal packaging in high-end fields are still irreplaceable. However, such packaging materials have the problem of sticking to the mold in the packaging mold, which affects the packaging quality, mold life and production efficiency, therefore, it is particularly important to provide a high-performance mold release agent in the process of semiconductor packaging.

[0003] Common mold release agents mainly include three categories of wax, silicone and organofluorine. Among them, the silicone mold release agent has achieved a good balance in performance, price and applicability - it has uniform film formation, smooth release, good temperature resistance, and moderate price, so it has become the most widely used mold release product in the current industrial field with outstanding comprehensive advantages.

[0004] In order to promote industrial upgrading and improve international competitiveness, people have higher requirements for domestic semiconductors, therefore, it is urgent to develop a mold release agent with high heat resistance, good mechanical properties, good release effect and excellent wear resistance to meet the needs of large-scale production. SUMMARY

[0005] In order to solve the problems mentioned in the background art, the present application provides a high-temperature stable mold release agent and a preparation method thereof.

[0006] A high-temperature stable mold release agent, comprising the following raw materials by weight: 18-22 parts of blended rubber, 6-8 parts of functionalized reinforcing agent, 2-4 parts of wear-resistant component, 4-5 parts of mold cleaning agent, 0.02-0.04 parts of crosslinking agent and 0.0006-0.0012 parts of polymerization inhibitor; The functionalized reinforcing agent is obtained by nucleophilic substitution reaction of 1-chloromethyl-3-trifluoromethylbenzene and 2-allylphenol to obtain a phenyl monomer, then by hydrosilylation reaction with triethoxysilane to obtain a modifier, and finally by hydrolysis condensation reaction with allyl triethoxysilane and KH-560; The wear-resistant component is prepared from hydroxypropyl-terminated polydimethylsiloxane modified nano-titanium dioxide.

[0007] A preparation method of a high-temperature stable mold release agent, comprising the following preparation steps: Step S1, weigh the raw materials, put the blended rubber into the internal mixer, and pre-mix to obtain a pre-mixed material; Step S2, to the premix, sequentially add functional reinforcing agent, wear-resistant component, mold release agent, crosslinking agent and polymerization inhibitor, continue to mix 8-12min, discharge, extend pressure forming, get high temperature stable mold release agent.

[0008] Further, in the step S1, the blended rubber is mixed by natural rubber and perfluoroether rubber in a mass ratio of 3.5-4.5:1.

[0009] Further, in the step S1, the premixing temperature is 50-60℃, and the mixing time is 16-20min.

[0010] Further, in the step S1, the mold release agent is mixed by triethanolamine, ethylene glycol phenyl ether and diethylene glycol butyl ether in a mass ratio of 1:0.8-1.2:0.9-1.1.

[0011] Further, in the step S2, the mixing temperature is 120-140℃.

[0012] Further, in the step S2, the crosslinking agent is azobisisobutyronitrile or benzoyl peroxide.

[0013] Further, in the step S2, the polymerization inhibitor is hydroquinone.

[0014] Further, the functional reinforcing agent is prepared by the following steps: Step A1, under nitrogen protection, 1-chloromethyl-3-trifluoromethyl benzene, 2-allyl phenol, triethylamine and toluene are added into anhydrous DMF, stirred uniformly, heated to reflux for 6-8h, filtered, rotary evaporated, the rotary evaporated product is redissolved in acetone, filtered, the filtrate is rotary evaporated to obtain the phenyl monomer, wherein the mass ratio of 1-chloromethyl-3-trifluoromethyl benzene, 2-allyl phenol, triethylamine, toluene, anhydrous DMF and acetone is 2.7-5.4:2-4:0.3-0.5:16-20:30-40:18-22, in the above reaction process, triethylamine is used as an acid binding agent, anhydrous DMF is used as a solvent, and the phenyl monomer is obtained by nucleophilic substitution reaction; Step A2, under nitrogen protection, the phenyl monomer is added into toluene, heated to 52-56℃, stirred uniformly, then cast catalyst is added, continue to stir for 0.5-0.7h, then triethoxysilane is added, heated to 72-76℃, reacted for 18-22h, reduced pressure distillation to obtain the modifier, wherein the mass ratio of the phenyl monomer, triethoxysilane, cast catalyst and toluene is 4-6:1.8-2.6:0.5-0.8:40-50, in the above reaction process, the phenyl monomer and triethoxysilane occur silicon hydrogen addition to prepare the modifier; Step A3, the modifier, allyl triethoxysilane and KH-560 are added into anhydrous toluene, stirred uniformly, and the aqueous hydrochloric acid solution is added dropwise, after dropping, the hydrolysis reaction is carried out at room temperature for 0.6-0.8h, the temperature is increased to 58-62℃, and the reaction is stirred for 5.6-6.4h, then the layers are separated after standing, washed, and rotary evaporated to obtain the prepolymer monomer, and the polymerization reaction is carried out at 146-152℃ for 1.2-1.4h to obtain the functional reinforcing agent, wherein the mass ratio of the modifier, allyl triethoxysilane, KH-560, anhydrous toluene and the aqueous hydrochloric acid solution is 1.6-2.2:1:0.6-0.8:8-10:5-7, and in the above reaction process, the modifier and allyl triethoxysilane undergo hydrolysis and condensation reaction to obtain the functional reinforcing agent.

[0015] Further, the wear-resistant component is prepared by the following steps: The tetrabutyl titanate and anhydrous ethanol are mixed uniformly, and then the mixture of anhydrous ethanol, the aqueous hydrochloric acid solution and the hydroxypropyl-terminated polydimethylsiloxane is added dropwise, the temperature is increased to 50-60℃, and the reaction is stirred for 3.4-4.2h to obtain the wear-resistant component, wherein the mass ratio of the tetrabutyl titanate, the anhydrous ethanol and the mixture is 0.8-1.2:16-20:40, and in the mixture, the mass ratio of the anhydrous ethanol, the aqueous hydrochloric acid solution and the hydroxypropyl-terminated polydimethylsiloxane is 18-22:3-4:0.2-0.4.

[0016] Further, the mass fraction of the aqueous hydrochloric acid solution is 0.6-0.8%.

[0017] Compared with the prior art, the present application has the following beneficial effects: In order to improve the heat resistance, mechanical properties, release effect and wear resistance of the release agent, the present application starts from two aspects, one is to add the functional reinforcing agent, the functional reinforcing agent contains -Si-O-Si bond, benzene ring, trifluoromethyl and unsaturated double bond, the presence of -Si-O-Si bond, on the one hand, together with the rigid benzene ring, improves the heat resistance of the release agent, on the other hand, forms a polysiloxane-rubber-based block copolymer in the release agent, so that the release agent has the release effect and heat resistance of organosiloxane, the trifluoromethyl has a lower surface energy, which can improve the release effect and heat resistance of the release agent, and the presence of unsaturated double bond can chemically crosslink with the natural rubber in the blended rubber, thereby improving the mechanical properties and heat resistance of the release agent; the other is to add the wear-resistant component, on the one hand, the excellent physical properties of nano titanium dioxide are utilized to further improve the mechanical properties and heat resistance of the release agent, and on the other hand, the hydroxypropyl-terminated polydimethylsiloxane grafted on the surface of nano titanium dioxide has a polysiloxane structure, which is rigid and heat-resistant, and when it is introduced into the release agent, it can play a synergistic role with the functional reinforcing agent to improve the heat resistance, mechanical properties, release effect and wear resistance of the release agent. DETAILED DESCRIPTION

[0018] In order to make the embodiments of the present application more easily understood, the present application will be described in detail below with specific examples, which are only illustrative and not limited to the scope of the present application.

[0019] The present application will be further described below in conjunction with examples.

[0020] The main raw materials used in the examples and the content of their components are shown as follows: The Kast catalyst is a platinum gold catalyst produced by Platinum World Company, with CAS number 68478-92-2; the natural rubber is commercially available from Ling Shou County Beiqiu Building Material Sales Co., Ltd.; the perfluoroether rubber is commercially available from Hubei Xinyu Hong Biological Medicine Technology Co., Ltd., with CAS number XYH; the hydroxypropyl-terminated polydimethylsiloxane is commercially available from Guangdong Wengjiang Chemical Reagent Co., Ltd., with CAS number 104780-66-7.

[0021] Example 1 The present embodiment provides a high-temperature stable mold release agent, which comprises the following raw materials by weight: 18 parts of blended rubber, 6 parts of functionalized reinforcing agent, 2 parts of wear-resistant component, 4 parts of mold cleaning agent, 0.02 parts of azobisisobutyronitrile and 0.0006 parts of hydroquinone, wherein the blended rubber is obtained by mixing natural rubber and perfluoroether rubber at a mass ratio of 3.5:1, and the mold cleaning agent is obtained by mixing triethanolamine, ethylene glycol phenyl ether and diethylene glycol butyl ether at a mass ratio of 1:0.8:0.9. A preparation method of a high-temperature stable mold release agent, comprising the following steps: Step S1, weigh the raw materials, put the blended rubber into the internal mixer, mix at 50℃ for 20min to obtain a premix; Step S2, add the functionalized reinforcing agent, wear-resistant component, mold cleaning agent, azobisisobutyronitrile and hydroquinone into the premix in sequence, continue to mix at 120℃ for 12min, discharge, and extend the pressure to form a high-temperature stable mold release agent; The functionalized reinforcing agent is prepared by the following steps: Step A1, under nitrogen protection, 1-chloromethyl-3-trifluoromethylbenzene, 2-allylphenol, triethylamine and toluene are added into anhydrous DMF, stirred at a speed of 600rpm for 26min until uniform, the speed is kept unchanged while the temperature is raised to reflux, continue to stir for 6h, filter, the filtrate is rotary evaporated at a rotary evaporation temperature of 82℃ to remove anhydrous DMF, the rotary evaporation product is redissolved in acetone, filtered to remove triethylamine hydrochloride, and then rotary evaporated at a rotary evaporation temperature of 66℃ to remove toluene and acetone to obtain a phenyl monomer, wherein the mass ratio of 1-chloromethyl-3-trifluoromethylbenzene, 2-allylphenol, triethylamine, toluene, anhydrous DMF and acetone is 2.7:2:0.3:16:30:18; Step A2, under the condition of nitrogen protection, the phenyl monomer was added into toluene, heated to 52℃, the stirring speed was controlled at 600 rpm, and stirred for 30 min until uniform, then the Karstedt catalyst was added, the stirring speed was kept unchanged, and stirring was continued for 0.7 h, then triethoxysilane was added, heated to 72℃, and reacted for 22 h, then toluene was removed by distillation under reduced pressure to obtain the modifier, wherein the mass ratio of the phenyl monomer, triethoxysilane, Karstedt catalyst and toluene was 4:1.8:0.5:40; Step A3, the modifier, allyl triethoxysilane and KH-560 were added into anhydrous toluene, stirred at a stirring speed of 680 rpm for 28 min until uniform, then a 0.6% mass fraction hydrochloric acid aqueous solution was added dropwise, and the dropping was completed within 5 min, after dropping, hydrolysis reaction was carried out at room temperature for 0.6 h, then heated to 58℃, and stirred for 6.4 h, then the anhydrous toluene was removed by standing and layering, then washed with water at 55℃ until neutral, and then constant weight was performed by rotary evaporation at 45℃ to obtain the prepolymer monomer, then polymerization reaction was carried out at 146℃, and the polymerization reaction time was 1.4 h to obtain the functional reinforcing agent, wherein the mass ratio of the modifier, allyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution was 1.6:1:0.6:8:5; The wear-resistant component was prepared by the following steps: The titanium tetrabutoxide and anhydrous ethanol were mixed at a stirring speed of 600 rpm for 22 min until uniform, then a mixture of anhydrous ethanol, a 0.6% mass fraction hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane was added dropwise, and the dropping was completed within 10 min, then heated to 50℃, the stirring speed was kept unchanged, and stirring reaction was carried out for 4.2 h to obtain the wear-resistant component, wherein the mass ratio of the titanium tetrabutoxide, anhydrous ethanol and the mixture was 0.8:16:40, and in the mixture, the mass ratio of the anhydrous ethanol, hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane was 18:3:0.2.

[0022] Example 2 The present embodiment provides a high-temperature stable mold release agent, which comprises the following raw materials by weight: 20 parts of blended rubber, 7 parts of functional reinforcing agent, 3 parts of wear-resistant component, 4.5 parts of mold cleaning agent, 0.03 parts of benzoyl peroxide and 0.0009 parts of hydroquinone, wherein the blended rubber is obtained by mixing natural rubber and perfluoroether rubber at a mass ratio of 4:1, and the mold cleaning agent is obtained by mixing triethanolamine, ethylene glycol phenyl ether and diethylene glycol butyl ether at a mass ratio of 1:1:1; A preparation method of a high-temperature stable mold release agent, comprising the following steps: Step S1, raw materials were weighed, and the blended rubber was put into a mixer, and pre-mixed at 55℃ for 18 min to obtain a pre-mixed material; Step S2, to the premix, sequentially add functional reinforcing agent, wear-resistant component, mold release agent, benzoyl peroxide and hydroquinone, control the temperature to 130℃, continue to mix for 10min, discharge, and extend pressure forming, get high temperature stable mold release agent; The functional reinforcing agent is prepared by the following steps: Step A1, under nitrogen protection, 1-chloromethyl-3-trifluoromethyl benzene, 2-allyl phenol, triethylamine and toluene are added into anhydrous DMF, stirring at a speed of 650rpm for 22min until uniform, the temperature is raised to reflux temperature, the stirring speed is kept unchanged, and the stirring reaction is continued for 7h, filtration, the filtrate, the filtrate is rotary evaporated to remove anhydrous DMF at a rotary evaporation temperature of 84℃, the rotary evaporation product is redissolved in acetone, the triethylamine hydrochloride is removed by filtration, and then the toluene and acetone are removed by rotary evaporation at a rotary evaporation temperature of 68℃, to obtain a phenyl monomer, wherein the mass ratio of 1-chloromethyl-3-trifluoromethyl benzene, 2-allyl phenol, triethylamine, toluene, anhydrous DMF and acetone is 4.05:3:0.4:18:35:20; Step A2, under nitrogen protection, the phenyl monomer is added into toluene, the temperature is raised to 54℃, stirring at a speed of 700rpm for 26min until uniform, then the Karstedt catalyst is added, the stirring speed is kept unchanged, and the stirring reaction is continued for 0.6h, then triethoxysilane is added, the temperature is raised to 74℃, and the reaction is carried out for 20h, then the toluene is removed by reduced pressure distillation, to obtain a modifier, wherein the mass ratio of the phenyl monomer, triethoxysilane, Karstedt catalyst and toluene is 5:2.2:0.65:45; Step A3, the modifier, allyl triethoxysilane and KH-560 are added into anhydrous toluene, stirring at a speed of 700rpm for 26min until uniform, then a mass fraction of 0.7% hydrochloric acid aqueous solution is added dropwise, which is controlled to be dropped within 5min, after dropping, the hydrolysis reaction is carried out at room temperature for 0.7h, the temperature is raised to 60℃, the stirring speed is kept unchanged, and the stirring reaction is continued for 6h, then the anhydrous toluene phase is removed by standing and layering, the toluene phase is washed with water at 60℃ until neutral, and then rotary evaporation is carried out at 50℃ until constant weight, to obtain a prepolymer monomer, which is subjected to polymerization reaction at 149℃, and the polymerization reaction time is 1.3h, to obtain a functional reinforcing agent, wherein the mass ratio of the modifier, allyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution is 1.9:1:0.7:9:6; The wear-resistant component is prepared by the following steps: The tetrabutyl titanate and anhydrous ethanol are mixed for 20 min under the control of the rotating speed of 640 rpm to be uniform, and then the mixed solution of anhydrous ethanol, the mass fraction of 0.7% hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane is added dropwise, which is controlled to be dropped in 10 min, the temperature is increased to 55℃, the rotating speed is kept unchanged, and the stirring reaction is carried out for 3.8 h to obtain the wear-resistant component, wherein the mass ratio of the tetrabutyl titanate, the anhydrous ethanol and the mixed solution is 1:18:40, and in the mixed solution, the mass ratio of the anhydrous ethanol, the hydrochloric acid aqueous solution and the hydroxypropyl-terminated polydimethylsiloxane is 20:3.5:0.3.

[0023] Example 3 The embodiment provides a high-temperature stable mold release agent, which comprises the following raw materials in parts by weight: 22 parts of blended rubber, 8 parts of functionalized reinforcing agent, 4 parts of wear-resistant component, 5 parts of mold cleaning agent, 0.04 parts of azobisisobutyronitrile and 0.0012 parts of hydroquinone, wherein the blended rubber is obtained by mixing natural rubber and perfluoroether rubber at a mass ratio of 4.5:1, and the mold cleaning agent is obtained by mixing triethanolamine, ethylene glycol phenyl ether and diethylene glycol butyl ether at a mass ratio of 1:1.2:1.1. A preparation method of a high-temperature stable mold release agent, comprising the following steps: Step S1, the raw materials are weighed, the blended rubber is put into a mixing mill, and pre-mixing is carried out at 60℃ for 16 min to obtain a pre-mixed material; Step S2, the functionalized reinforcing agent, the wear-resistant component, the mold cleaning agent, the azobisisobutyronitrile and the hydroquinone are sequentially added to the pre-mixed material, the temperature is controlled to be 140℃, and then mixing is continuously carried out for 8 min, the material is discharged, and pressure forming is carried out to obtain the high-temperature stable mold release agent; The functionalized reinforcing agent is obtained by the following steps: Step A1, under nitrogen protection, 1-chloromethyl-3-trifluoromethylbenzene, 2-allylphenol, triethylamine and toluene are added into anhydrous DMF, stirring is carried out at a rotating speed of 700 rpm for 18 min to be uniform, the temperature is increased to the reflux temperature, the rotating speed is kept unchanged, and stirring reaction is continuously carried out for 8 h, filtration is carried out, the filtrate is subjected to rotary evaporation to remove anhydrous DMF at a rotary evaporation temperature of 86℃, the rotary evaporation product is redissolved in acetone, triethylamine hydrochloride is removed by filtration, and then toluene and acetone are removed by rotary evaporation at a rotary evaporation temperature of 70℃ to obtain the phenyl monomer, wherein the mass ratio of 1-chloromethyl-3-trifluoromethylbenzene, 2-allylphenol, triethylamine, toluene, anhydrous DMF and acetone is 5.4:4:0.5:20:40:22; Step A2, under the condition of nitrogen protection, the phenyl monomer was added into toluene, heated to 56℃, the stirring speed was controlled at 800 rpm, and stirred for 22 min until uniform, then the Karstedt catalyst was added, the stirring speed was kept unchanged, and stirring was continued for 0.5 h, then triethoxysilane was added, heated to 76℃, and reacted for 18 h, then toluene was removed by distillation under reduced pressure to obtain the modifier, wherein the mass ratio of the phenyl monomer, triethoxysilane, Karstedt catalyst and toluene was 6:2.6:0.8:50; Step A3, the modifier, allyl triethoxysilane and KH-560 were added into anhydrous toluene, stirred for 24 min at a stirring speed of 720 rpm until uniform, then a 0.8% mass fraction hydrochloric acid aqueous solution was added dropwise, and the dropping was completed within 5 min, after dropping, hydrolysis reaction was carried out at room temperature for 0.8 h, then the stirring speed was kept unchanged, and stirring reaction was continued at 62℃ for 5.6 h, then the anhydrous toluene phase was removed after standing and layering, and the water was washed at 65℃ until neutral, then rotary evaporation was carried out at 55℃ until constant weight to obtain a prepolymer monomer, and the prepolymer monomer was subjected to polymerization reaction at 152℃ for 1.2 h to obtain the functional reinforcing agent, wherein the mass ratio of the modifier, allyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution was 2.2:1:0.8:10:7; The wear-resistant component was prepared by the following steps: Tetrabutyl titanate and anhydrous ethanol were mixed for 18 min at a stirring speed of 680 rpm until uniform, then a mixture of anhydrous ethanol, a 0.8% mass fraction hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane was added dropwise, the dropping was completed within 10 min, the stirring speed was kept unchanged, and stirring reaction was carried out at 60℃ for 3.4 h to obtain the wear-resistant component, wherein the mass ratio of tetrabutyl titanate, anhydrous ethanol and the mixture was 1.2:20:40, and the mass ratio of anhydrous ethanol, hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane in the mixture was 22:4:0.4.

[0024] Comparative Example 1 The difference between this comparative example and Example 1 was that, when the functional reinforcing agent was prepared, 1-chloromethyl-3-trifluoromethylbenzene was replaced by 4-(chloromethyl)benzoyl chloride, and the remaining steps and raw materials were implemented synchronously with Example 1. The functional reinforcing agent was prepared by the following steps: Step A1, under the protection of nitrogen, 4-(chloromethyl)benzoyl chloride, 2-allyl phenol, triethylamine and toluene were added into anhydrous DMF, stirred at 600 rpm for 26 min until uniform, heated to reflux temperature, maintained the same speed, continued to stir for 6 h, filtered, the filtrate was removed by rotary evaporation at 82°C, the rotary evaporation product was dissolved in acetone, filtered to remove triethylamine hydrochloride, the filtrate was removed by rotary evaporation at 66°C to remove toluene and acetone, and the phenyl monomer was obtained, wherein the mass ratio of 4-(chloromethyl)benzoyl chloride, 2-allyl phenol, triethylamine, toluene, anhydrous DMF and acetone was 2.7:2:0.3:16:30:18; Step A2, under the protection of nitrogen, the phenyl monomer was added into toluene, heated to 52°C, controlled the stirring speed at 600 rpm, stirred for 30 min until uniform, then added Koster catalyst, maintained the same speed, continued to stir for 0.7 h, then added triethoxysilane, heated to 72°C, reacted for 22 h, distilled under reduced pressure to remove toluene, and the modifier was obtained, wherein the mass ratio of the phenyl monomer, triethoxysilane, Koster catalyst and toluene was 4:1.8:0.5:40; Step A3, the modifier, allyl triethoxysilane and KH-560 were added into anhydrous toluene, stirred at 680 rpm for 28 min until uniform, then added 0.6% mass fraction hydrochloric acid aqueous solution dropwise, controlled the dropwise time within 5 min, after dropwise, hydrolysis reaction was carried out at room temperature for 0.6 h, heated to 58°C, stirred for 6.4 h, separated the layers to remove the anhydrous toluene phase, washed with 55°C water until neutral, and rotary evaporated at 45°C to constant weight, to obtain the prepolymer monomer, and the functional reinforcing agent was obtained by polymerization reaction at 146°C for 1.4 h, wherein the mass ratio of the modifier, allyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution was 1.6:1:0.6:8:5.

[0025] Comparative Example 2 The difference between this comparative example and Example 1 is that 2-allyl phenol is replaced by 4-propyl phenol in the same amount when preparing the functional reinforcing agent, and the remaining steps and raw materials are the same as Example 1. The functional reinforcing agent was prepared by the following steps: Step A1, under the protection of nitrogen, 1-chloromethyl-3-trifluoromethylbenzene, 4-propylphenol, triethylamine and toluene were added into anhydrous DMF, stirred at 600 rpm for 26 min until uniform, heated to reflux temperature, maintained the same speed, continued to stir for 6 h, filtered, the filtrate was removed by rotary evaporation at 82°C, the product was dissolved in acetone, filtered to remove triethylamine hydrochloride, and then removed by rotary evaporation at 66°C to remove toluene and acetone, to obtain a phenyl monomer, wherein the mass ratio of 1-chloromethyl-3-trifluoromethylbenzene, 4-propylphenol, triethylamine, toluene, anhydrous DMF and acetone was 2.7:2:0.3:16:30:18; Step A2, under the protection of nitrogen, the phenyl monomer was added to toluene, heated to 52°C, controlled the stirring speed at 600 rpm, stirred for 30 min until uniform, then added Koster catalyst, maintained the same speed, continued to stir for 0.7 h, then added triethoxysilane, heated to 72°C, reacted for 22 h, distilled under reduced pressure to remove toluene, to obtain a modifier, wherein the mass ratio of phenyl monomer, triethoxysilane, Koster catalyst and toluene was 4:1.8:0.5:40; Step A3, the modifier, allyl triethoxysilane and KH-560 were added into anhydrous toluene, stirred at 680 rpm for 28 min until uniform, added 0.6% mass fraction hydrochloric acid aqueous solution dropwise, controlled the dropwise time within 5 min, after dropwise, hydrolysis reaction at room temperature for 0.6 h, heated to 58°C, stirred for 6.4 h, separated the layers to remove the anhydrous toluene phase, washed with 55°C water until neutral, rotary evaporated at 45°C to constant weight, to obtain a prepolymer monomer, which was subjected to polymerization reaction at 146°C, the polymerization reaction time was 1.4 h, to obtain a functional reinforcing agent, wherein the mass ratio of modifier, allyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution was 1.6:1:0.6:8:5.

[0026] Comparative Example 3 The difference between this comparative example and Example 1 is that, when preparing the functional reinforcing agent, the allyl triethoxysilane was replaced with an equal amount of methyl triethoxysilane, and the remaining steps and raw materials were implemented synchronously with Example 1. The functional reinforcing agent was prepared by the following steps: Step A1, under the protection of nitrogen, 1-chloromethyl-3-trifluoromethylbenzene, 2-allylphenol, triethylamine and toluene were added into anhydrous DMF, stirred at 600 rpm for 26 min until uniform, heated to reflux temperature, maintained the same speed, continued to stir the reaction for 6 h, filtered, the filtrate was removed by rotary evaporation at a rotary evaporation temperature of 82°C, the product was redissolved in acetone, filtered to remove triethylamine hydrochloride, and then removed by rotary evaporation at a rotary evaporation temperature of 66°C to remove toluene and acetone, to obtain a phenyl monomer, wherein the mass ratio of 1-chloromethyl-3-trifluoromethylbenzene, 2-allylphenol, triethylamine, toluene, anhydrous DMF and acetone is 2.7:2:0.3:16:30:18; Step A2, under the protection of nitrogen, the phenyl monomer was added to toluene, heated to 52°C, controlled the stirring speed at 600 rpm, stirred for 30 min until uniform, then added Koster catalyst, maintained the same speed, continued to stir for 0.7 h, then added triethoxysilane, heated to 72°C, reacted for 22 h, distilled under reduced pressure to remove toluene, to obtain a modifier, wherein the mass ratio of the phenyl monomer, triethoxysilane, Koster catalyst and toluene is 4:1.8:0.5:40; Step A3, the modifier, methyl triethoxysilane and KH-560 were added into anhydrous toluene, stirred at 680 rpm for 28 min until uniform, added 0.6% hydrochloric acid aqueous solution dropwise, controlled to drop within 5 min, after dropping, hydrolysis reaction at room temperature for 0.6 h, heated to 58°C, stirred for 6.4 h, separated the layers to remove the anhydrous toluene phase, washed with 55°C water until neutral, rotary evaporated at 45°C to constant weight, to obtain a prepolymer monomer, polymerized at 146°C, the polymerization reaction time was 1.4 h, to obtain a functional reinforcing agent, wherein the mass ratio of the modifier, methyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution is 1.6:1:0.6:8:5.

[0027] Comparative Example 4 The difference between this comparative example and Example 1 is that when preparing the wear-resistant component, the hydroxypropyl-terminated polydimethylsiloxane is replaced with polydimethylsiloxane in equal mass, and the remaining steps and raw materials are implemented synchronously with Example 1. The wear-resistant component was prepared by the following steps: Tetrabutyl titanate and anhydrous ethanol were mixed at a stirring speed of 600 rpm for 22 min until uniform, then a mixed solution of anhydrous ethanol, 0.6% hydrochloric acid aqueous solution and polydimethylsiloxane was added dropwise, controlled to drop within 10 min, heated to 50°C, maintained the same speed, stirred for 4.2 h, to obtain a wear-resistant component, wherein the mass ratio of tetrabutyl titanate, anhydrous ethanol and the mixed solution is 0.8:16:40, in the mixed solution, the mass ratio of anhydrous ethanol, hydrochloric acid aqueous solution and polydimethylsiloxane is 18:3:0.2 Performance test High-temperature stable mold release agents were prepared according to Examples 1-3 and Comparative Examples 1-4, respectively, and performance tests were sequentially performed.

[0028] 1. Mechanical property test The tensile strength and tear strength of the samples were measured, respectively, wherein the tensile strength test was specified with reference to the standard GB / T 528-2009, and the tensile speed was controlled at 450 mm / min, and the tear strength test was specified with reference to GB / T 529-2008; 2. Mold cleaning effect test Taking commercially available Kraft K-9741 black epoxy resin potting adhesive as an example, 14 groups of semiconductor packaging molds reaching the same number of mold sealing operations were taken, i.e. after the mold reaches a fixed number of packaging operations in production, mold cleaning is required, high-temperature stable mold release agents prepared by Examples 1-3 and Comparative Examples 1-4 were used to fill the semiconductor packaging molds, and after hot pressing at 200°C for 15s, the mold release was taken out, and whether there was residual dirt on the surface and in the mold cavity was observed, and repeated cleaning was performed until clean, the number of mold cleaning required was recorded, and the average value was obtained by removing the extreme value; 4. Wear resistance test An Akron abrasion tester was used for testing, and the test standard was referred to GB / T 1689-2014; The specific test results are shown in Table 1. Table 1 Performance test of mold release agents prepared by Examples 1-3 and Comparative Examples 1-4 As can be seen from Table 1, compared with Comparative Example 1-4, the high-temperature stable mold release agent prepared by Example 1-3 has more excellent heat resistance, mechanical properties, mold release effect and wear resistance.

[0029] The specific embodiments are merely an explanation of the present application, and are not a limitation of the present application. Those skilled in the art can make modifications to the embodiments without creative contribution after reading the specification, and the modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A high temperature stable mold release agent characterized in that, The functional reinforcing agent is prepared by the following steps: Step A1, under nitrogen protection, 1-chloromethyl-3-trifluoromethyl benzene, 2-allyl phenol, triethylamine and toluene are added into anhydrous DMF, stirred uniformly, heated to reflux for 6-8h, filtered, rotary evaporated, the rotary evaporated product is dissolved in acetone, filtered, the filtrate is rotary evaporated to obtain the phenyl monomer; Step A2, under nitrogen protection, the phenyl monomer is added into toluene, heated to 52-56℃, stirred uniformly, then Kast catalyst is added, continue to stir for 0.5-0.7h, then triethoxysilane is added, heated to 72-76℃, reacted for 18-22h, reduced pressure distillation to obtain the modifier; 2. A high temperature stable mold release agent according to claim 1, wherein, Step A3, the modifier, allyl triethoxysilane and KH-560 are added into anhydrous toluene, stirred uniformly, then hydrochloric acid aqueous solution is added dropwise, after dropping, hydrolysis reaction is carried out at room temperature for 0.6-0.8h, heated to 58-62℃, stirred for 5.6-6.4h, static stratification, washed, rotary evaporated to obtain the prepolymer monomer, polymerization reaction is carried out at 146-152℃ for 1.2-1.4h to obtain the functional reinforcing agent. In step A1, the mass ratio of 1-chloromethyl-3-trifluoromethyl benzene, 2-allyl phenol, triethylamine, toluene, anhydrous DMF and acetone is 2.7-5.4:2-4:0.3-0.5:16-20:30-40:18-22. In step A2, the mass ratio of the phenyl monomer, triethoxysilane, Kast catalyst and toluene is 4-6:1.8-2.6:0.5-0.8:40-50. In step A3, the mass ratio of the modifier, allyl triethoxysilane, KH-560, anhydrous toluene and hydrochloric acid aqueous solution is 1.6-2.2:1:0.6-0.8:8-10:5-7.

3. A high temperature stable mold release agent according to claim 2, wherein The wear-resistant component is prepared by the following steps:

4. A high temperature stable mold release agent according to claim 2, wherein The tetrabutyl titanate and anhydrous ethanol are mixed uniformly, then the mixed solution of anhydrous ethanol, hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane is added dropwise, heated to 50-60℃, stirred for 3.4-4.2h to obtain the wear-resistant component.

5. A high temperature stable mold release agent according to claim 2, wherein The mass ratio of the tetrabutyl titanate, anhydrous ethanol and the mixed solution is 0.8-1.2:16-20:40, and the mass ratio of anhydrous ethanol, hydrochloric acid aqueous solution and hydroxypropyl-terminated polydimethylsiloxane in the mixed solution is 18-22:3-4:0.2-0.

4.

6. A high temperature stable mold release agent according to claim 1, wherein ​ ​ 7. A high temperature stable mold release agent according to claim 6, wherein ​ 8. A method for preparing the high-temperature stable mold release agent according to any one of claims 1-7, comprising the following steps: Step S1, weighing the raw materials, putting the blended rubber into the internal mixer, pre-mixing, and obtaining the pre-mixed material; Step S2, adding the functional reinforcing agent, wear-resistant component, mold cleaning agent, crosslinking agent and polymerization inhibitor into the pre-mixed material in sequence, continuing to mix for 8-12 min, discharging, and extending and forming to obtain the high-temperature stable mold release agent.

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