A processing technique for high transparent resin
By using self-made resin mixtures and modifiers, combined with precise processing techniques, the problems of air bubbles and mold defects in high-transparency molded grid resin were solved, improving the optical and mechanical properties of the product.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ZHENJIANG LEADER COMPOSITE CO LTD
- Filing Date
- 2023-07-07
- Publication Date
- 2026-06-05
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Figure BDA0004326424720000181 
Figure BDA0004326424720000191
Abstract
Description
Technical Field
[0001] This invention relates to the field of grid resin technology, and more specifically to a processing technology for a high-transparency resin. Background Technology
[0002] High-transparency molding grating resin is a resin material with high transparency and excellent mechanical properties, widely used in optics, electronics, automotive, and other industries. It excels in light transmittance, heat resistance, chemical resistance, and strength, thus replacing traditional glass materials in many applications.
[0003] In past processing techniques, common methods included injection molding, extrusion molding, and calendering. However, achieving high transparency in molded grating resin products remains a challenge. The main issues are as follows:
[0004] 1. Bubbles and defects: During the injection molding process, high-transparency resins are prone to generating bubbles and other defects, which reduces the optical transparency of the product.
[0005] 2. Mold surface quality: Defects and unevenness on the mold surface will affect the optical quality of resin products.
[0006] Therefore, the processing technology for high-transparency molding grating resin needs to be improved to address the above-mentioned issues in order to enhance the optical transparency and mechanical properties of the product.
[0007] The present invention aims to overcome the problems existing in the prior art and provide a processing technology for high-transparency molding grating resin to obtain high-quality resin products. Summary of the Invention
[0008] The purpose of this invention is to provide a processing technology for highly transparent resin to solve the problems mentioned in the background art.
[0009] To achieve the above objectives, the present invention provides the following technical solution:
[0010] A processing method for a highly transparent resin includes the following steps:
[0011] (1) Prepare the homemade resin mixture;
[0012] (2) Add appropriate additives to the homemade resin mixture;
[0013] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0014] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0015] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0016] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0017] (7) Cool the mold to allow the resin to solidify rapidly;
[0018] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0019] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0020] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0021] By weight, take 20-30 parts of polymethyl methacrylate, 10-20 parts of homemade polycarbonate, 5-8 parts of homemade resin, and 1-2 parts of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, homemade polycarbonate, homemade resin, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 10-20 minutes at a temperature of 200-300℃ and a speed of 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at a temperature of 200-300℃ and a pressure of 10-20 MPa. After cooling, crush the mixture to obtain the homemade resin mixture.
[0022] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0023] Preferably, the specific preparation process of the self-made polycarbonate is as follows:
[0024] 1) By weight, take 1-2 parts of 4-methoxy-4'-hydroxyazobenzene, 1-2 parts of triethylamine, 1-2 parts of p-fluorobenzoyl chloride, and 200-300 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt-ice bath. Then, add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 24-48 hours. Remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 5-8 times, and then wash it repeatedly with distilled water and filter it 5-8 times to obtain a filter cake. Then, recrystallize the filter cake with a mixed solution of acetone / ethanol at a volume ratio of 3:5 to obtain the modifier.
[0025] 2) By weight, take 2-3 parts of modifier, 20-30 parts of polycarbonate and 2-3 parts of pentaerythritol stearate. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 200-300℃ to obtain the self-made polycarbonate.
[0026] Preferably, the specific preparation process of the self-made resin is as follows:
[0027] 1) By weight, take 5-10 parts of 4,4'-dihydroxydiphenyl sulfone, 2-3 parts of 4,4'-dichlorodiphenyl sulfone, 2-3 parts of 4,4'-difluorobenzophenone, 2-3 parts of 3,4'-difluorobenzophenone, 2-3 parts of 3-fluoro-4'-chlorobenzophenone, 100-120 parts of sulfone, 1-2 parts of potassium bicarbonate, and 1-2 parts of sodium carbonate. '-Chlorobenzophenone and sulfone were placed in a reactor equipped with a nitrogen gas pipe, a condenser, and a stirrer. The mixture was stirred to dissolve the monomers. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 180-200°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 230-260°C and kept at a constant temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained.
[0028] 2) Mix the polymer powder with acetone at a mass ratio of 1:10-1:20, boil for 2-3 hours, repeat this treatment 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
[0029] Preferably, the pressure in step (6) is 10-20 MPa and the temperature is 200-400 °C.
[0030] In summary, due to the adoption of the above-mentioned technologies, the beneficial effects of this invention are:
[0031] (1) In this invention, by adding self-made polycarbonate, firstly, p-fluorobenzoyl chloride is introduced into 4-methoxy-4'-hydroxyazobenzene through reaction to obtain a modifier. During the mixing process with polycarbonate, the carbon-oxygen double bond in the modifier can interact with the carbon-oxygen double bond of polycarbonate through dipole-dipole interaction, thereby weakening the interaction of polycarbonate molecular chains, improving the flow of the product, and improving the fluidity of the components in the system, so that the components in the system can be fully mixed, thereby improving the mechanical properties and transparency of the product. At the same time, due to the addition of the modifier, the distance between the blended molecular chains of the modifier and polycarbonate is reduced, so that the orientation of the local segments of the polycarbonate molecular chain inhibits the crack propagation of the material during the stretching process, so that the crack direction is hindered and shifted to the side, strengthening the energy dissipation, thereby enhancing the tensile strength of the product.
[0032] (2) By adding self-made resin, the present invention firstly addresses the issue that unmodified polyarylether sulfone is an amorphous polymer with entangled molecular chains. Due to the rigid structure of its molecular chains, the entanglement between rigid chains is not easily resolved, making it difficult for the entire chain of macromolecules to move, resulting in a high melting temperature and reduced fluidity. After the introduction of ketone groups, since the ketone groups in the molecular chains are coplanar with the benzene rings, there is a certain interaction force between the molecular chains, which can break the entanglement between the polyarylether sulfone molecular chains. Furthermore, since the content of ketone groups in the molecular chains is relatively small, the π bond force between the molecular chains is weak. At this time, the decrease in the entanglement between the polyarylether sulfone molecular chains plays a dominant role in the effect on the fluidity of the polymer, thus improving the fluidity of the polymer. This increases the fluidity of the system, allowing the components in the system to be mixed more thoroughly, reducing the generation of bubbles. At the same time, the increased fluidity allows the components in the system to be better filled into the mold, avoiding the influence of defects and unevenness on the surface of the mold on the light transmittance of the resin product. Detailed Implementation
[0033] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention is not intended to limit the scope of the claimed invention, but merely to represent selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0034] Example 1
[0035] A processing method for a highly transparent resin includes the following steps:
[0036] (1) Prepare the homemade resin mixture;
[0037] (2) Add appropriate additives to the homemade resin mixture;
[0038] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0039] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0040] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0041] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0042] (7) Cool the mold to allow the resin to solidify rapidly;
[0043] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0044] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0045] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0046] By weight, take 20 parts of polymethyl methacrylate, 20 parts of homemade polycarbonate, 8 parts of homemade resin, and 1 part of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, homemade polycarbonate, homemade resin, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 20 minutes at 300°C and 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at 300°C and 10 MPa. After cooling and crushing, obtain the homemade resin mixture.
[0047] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0048] Preferably, the specific preparation process of the self-made polycarbonate is as follows:
[0049] 1) By weight, take 1 part of 4-methoxy-4'-hydroxyazobenzene, 2 parts of triethylamine, 2 parts of p-fluorobenzoyl chloride, and 300 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt ice bath. Then add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 48 hours. Remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 5 times, and then wash it repeatedly with distilled water and filter it 5 times to obtain a filter cake. Then recrystallize the filter cake with a mixed solution of acetone / ethanol with a volume ratio of 3:5 to obtain the modifier.
[0050] 2) By weight, take 2 parts of modifier, 20 parts of polycarbonate and 2 parts of pentaerythritol stearate. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 300°C to obtain the self-made polycarbonate.
[0051] Preferably, the specific preparation process of the self-made resin is as follows:
[0052] 1) By weight, take 10 parts of 4,4'-dihydroxydiphenyl sulfone, 2 parts of 4,4'-dichlorodiphenyl sulfone, 2 parts of 4,4'-difluorobenzophenone, 2 parts of 3,4'-difluorobenzophenone, 3 parts of 3-fluoro-4'-chlorobenzophenone, 100 parts of sulfone, 2 parts of potassium bicarbonate, and 1 part of sodium carbonate. Combine the following ingredients: 4,4'-dihydroxydiphenyl sulfone, 4,4'-dichlorodiphenyl sulfone, 4,4'-difluorobenzophenone, 3,4'-difluorobenzophenone, and 3-fluoro-4'-chlorodiphenyl sulfone. Methyl ketone and sulfone were placed in a reactor equipped with a nitrogen gas pipe, a condenser, and a stirrer. The mixture was stirred and dissolved. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 200°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 260°C and kept at that temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained.
[0053] 2) Mix the polymer powder with acetone at a mass ratio of 1:20, boil for 2 hours, repeat this process 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
[0054] Preferably, the pressure in step (6) is 10-20 MPa and the temperature is 200-400 °C.
[0055] Example 2
[0056] A processing method for a highly transparent resin includes the following steps:
[0057] (1) Prepare the homemade resin mixture;
[0058] (2) Add appropriate additives to the homemade resin mixture;
[0059] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0060] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0061] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0062] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0063] (7) Cool the mold to allow the resin to solidify rapidly;
[0064] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0065] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0066] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0067] By weight, take 26 parts of polymethyl methacrylate, 15 parts of self-made polycarbonate, 6 parts of self-made resin, and 2 parts of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, self-made polycarbonate, self-made resin, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 15 minutes at 300°C and 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at 300°C and 10 MPa. After cooling and crushing, obtain the self-made resin mixture.
[0068] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0069] Preferably, the specific preparation process of the self-made polycarbonate is as follows:
[0070] 1) By weight, take 2 parts of 4-methoxy-4'-hydroxyazobenzene, 1 part of triethylamine, 2 parts of p-fluorobenzoyl chloride, and 300 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt-ice bath. Then, add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 48 hours. Then, remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 6 times, and then wash it repeatedly with distilled water and filter it 6 times to obtain a filter cake. Then, recrystallize the filter cake with a mixed solution of acetone / ethanol with a volume ratio of 3:5 to obtain the modifier.
[0071] 2) By weight, take 2 parts of modifier, 30 parts of polycarbonate and 3 parts of pentaerythritol stearate. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 300°C to obtain the self-made polycarbonate.
[0072] Preferably, the specific preparation process of the self-made resin is as follows:
[0073] 1) By weight, take 6 parts of 4,4'-dihydroxydiphenyl sulfone, 3 parts of 4,4'-dichlorodiphenyl sulfone, 2 parts of 4,4'-difluorobenzophenone, 3 parts of 3,4'-difluorobenzophenone, 2 parts of 3-fluoro-4'-chlorobenzophenone, 100 parts of sulfone, 2 parts of potassium bicarbonate, and 1 part of sodium carbonate. Combine the following ingredients: 4,4'-dihydroxydiphenyl sulfone, 4,4'-dichlorodiphenyl sulfone, 4,4'-difluorobenzophenone, 3,4'-difluorobenzophenone, and 3-fluoro-4'-chlorodiphenyl sulfone. Methyl ketone and sulfone were placed in a reactor equipped with a nitrogen purging pipe, a condenser, and a stirrer. The mixture was stirred and dissolved. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 180°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 230°C and kept at that temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained.
[0074] 2) Mix the polymer powder with acetone at a mass ratio of 1:20, boil for 3 hours, repeat this treatment 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
[0075] Preferably, the pressure in step (6) is 16 MPa and the temperature is 300 °C.
[0076] Example 3
[0077] A processing method for a highly transparent resin includes the following steps:
[0078] (1) Prepare the homemade resin mixture;
[0079] (2) Add appropriate additives to the homemade resin mixture;
[0080] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0081] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0082] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0083] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0084] (7) Cool the mold to allow the resin to solidify rapidly;
[0085] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0086] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0087] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0088] By weight, take 20 parts of polymethyl methacrylate, 18 parts of homemade polycarbonate, 5 parts of homemade resin, and 2 parts of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, homemade polycarbonate, homemade resin, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 10 minutes at 300°C and 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at 300°C and 10 MPa. After cooling and crushing, obtain the homemade resin mixture.
[0089] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0090] Preferably, the specific preparation process of the self-made polycarbonate is as follows:
[0091] 1) By weight, take 2 parts of 4-methoxy-4'-hydroxyazobenzene, 2 parts of triethylamine, 2 parts of p-fluorobenzoyl chloride, and 280 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt-ice bath. Then, add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 36 hours. Then, remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 6 times, and then wash it repeatedly with distilled water and filter it 6 times to obtain a filter cake. Then, recrystallize the filter cake with a mixed solution of acetone / ethanol with a volume ratio of 3:5 to obtain the modifier.
[0092] 2) Take 3 parts modifier, 20 parts polycarbonate and 2 parts pentaerythritol stearate by weight. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 300°C to obtain the self-made polycarbonate.
[0093] Preferably, the specific preparation process of the self-made resin is as follows:
[0094] 1) By weight, take 8 parts of 4,4'-dihydroxydiphenyl sulfone, 3 parts of 4,4'-dichlorodiphenyl sulfone, 3 parts of 4,4'-difluorobenzophenone, 2 parts of 3,4'-difluorobenzophenone, 3 parts of 3-fluoro-4'-chlorobenzophenone, 120 parts of sulfone, 1 part of potassium bicarbonate, and 1 part of sodium carbonate. Combine the following ingredients: 4,4'-dihydroxydiphenyl sulfone, 4,4'-dichlorodiphenyl sulfone, 4,4'-difluorobenzophenone, 3,4'-difluorobenzophenone, and 3-fluoro-4'-chlorodiphenyl sulfone. Methyl ketone and sulfone were placed in a reactor equipped with a nitrogen purging pipe, a condenser, and a stirrer. The mixture was stirred and dissolved. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 200°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 260°C and kept at that temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained.
[0095] 2) Mix the polymer powder with acetone at a mass ratio of 1:20, boil for 3 hours, repeat this treatment 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
[0096] Preferably, the pressure in step (6) is 20 MPa and the temperature is 300 °C.
[0097] Comparative Example 1
[0098] A processing method for a highly transparent resin includes the following steps:
[0099] (1) Prepare the homemade resin mixture;
[0100] (2) Add appropriate additives to the homemade resin mixture;
[0101] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0102] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0103] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0104] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0105] (7) Cool the mold to allow the resin to solidify rapidly;
[0106] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0107] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0108] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0109] By weight, take 20 parts of polymethyl methacrylate, 18 parts of polycarbonate, 5 parts of self-made resin, and 2 parts of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, polycarbonate, self-made resin, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 10 minutes at 300°C and 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at 300°C and 10 MPa. After cooling and crushing, the self-made resin mixture is obtained.
[0110] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0111] Preferably, the specific preparation process of the self-made resin is as follows:
[0112] 1) By weight, take 8 parts of 4,4'-dihydroxydiphenyl sulfone, 3 parts of 4,4'-dichlorodiphenyl sulfone, 3 parts of 4,4'-difluorobenzophenone, 2 parts of 3,4'-difluorobenzophenone, 3 parts of 3-fluoro-4'-chlorobenzophenone, 120 parts of sulfone, 1 part of potassium bicarbonate, and 1 part of sodium carbonate. Combine the following ingredients: 4,4'-dihydroxydiphenyl sulfone, 4,4'-dichlorodiphenyl sulfone, 4,4'-difluorobenzophenone, 3,4'-difluorobenzophenone, and 3-fluoro-4'-chlorodiphenyl sulfone. Methyl ketone and sulfone were placed in a reactor equipped with a nitrogen purging pipe, a condenser, and a stirrer. The mixture was stirred and dissolved. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 200°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 260°C and kept at that temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained.
[0113] 2) Mix the polymer powder with acetone at a mass ratio of 1:20, boil for 3 hours, repeat this treatment 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
[0114] Preferably, the pressure in step (6) is 20 MPa and the temperature is 300 °C.
[0115] Comparative Example 2
[0116] A processing method for a highly transparent resin includes the following steps:
[0117] (1) Prepare the homemade resin mixture;
[0118] (2) Add appropriate additives to the homemade resin mixture;
[0119] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0120] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0121] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0122] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0123] (7) Cool the mold to allow the resin to solidify rapidly;
[0124] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0125] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0126] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0127] By weight, take 20 parts of polymethyl methacrylate, 18 parts of homemade polycarbonate, and 2 parts of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, homemade polycarbonate, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 10 minutes at 300°C and 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at 300°C and 10 MPa. After cooling and crushing, the homemade resin mixture is obtained.
[0128] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0129] Preferably, the specific preparation process of the self-made polycarbonate is as follows:
[0130] 1) By weight, take 2 parts of 4-methoxy-4'-hydroxyazobenzene, 2 parts of triethylamine, 2 parts of p-fluorobenzoyl chloride, and 280 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt-ice bath. Then, add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 36 hours. Then, remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 6 times, and then wash it repeatedly with distilled water and filter it 6 times to obtain a filter cake. Then, recrystallize the filter cake with a mixed solution of acetone / ethanol with a volume ratio of 3:5 to obtain the modifier.
[0131] 2) Take 3 parts modifier, 20 parts polycarbonate and 2 parts pentaerythritol stearate by weight. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 300°C to obtain the self-made polycarbonate.
[0132] Preferably, the pressure in step (6) is 20 MPa and the temperature is 300 °C.
[0133] Comparative Example 3
[0134] A processing method for a highly transparent resin includes the following steps:
[0135] (1) Prepare the homemade resin mixture;
[0136] (2) Add appropriate additives to the homemade resin mixture;
[0137] (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities;
[0138] (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state;
[0139] (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality;
[0140] (6) Inject the molten homemade resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the homemade resin mixture fully fills the mold cavity to form the product;
[0141] (7) Cool the mold to allow the resin to solidify rapidly;
[0142] (8) Open the mold and remove the molded high-transparency molded grid resin product;
[0143] (9) Post-processing of the molded product, namely deburring, trimming edges and polishing.
[0144] Preferably, the preparation steps of the self-made resin mixture in step (1) are as follows:
[0145] By weight, take 20 parts of polymethyl methacrylate, 18 parts of self-made polycarbonate, and 5 parts of self-made resin. Place the polymethyl methacrylate, self-made polycarbonate, and self-made resin in a mixer and mix for 10 minutes at 300°C and 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at 300°C and 10 MPa. After cooling and crushing, the self-made resin mixture is obtained.
[0146] Preferably, the additives in step (2) include UV stabilizers and antistatic agents.
[0147] Preferably, the specific preparation process of the self-made polycarbonate is as follows:
[0148] 1) By weight, take 2 parts of 4-methoxy-4'-hydroxyazobenzene, 2 parts of triethylamine, 2 parts of p-fluorobenzoyl chloride, and 280 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt-ice bath. Then, add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 36 hours. Then, remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 6 times, and then wash it repeatedly with distilled water and filter it 6 times to obtain a filter cake. Then, recrystallize the filter cake with a mixed solution of acetone / ethanol with a volume ratio of 3:5 to obtain the modifier.
[0149] 2) Take 3 parts modifier, 20 parts polycarbonate and 2 parts pentaerythritol stearate by weight. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 300°C to obtain the self-made polycarbonate.
[0150] Preferably, the specific preparation process of the self-made resin is as follows:
[0151] 1) By weight, take 8 parts of 4,4'-dihydroxydiphenyl sulfone, 3 parts of 4,4'-dichlorodiphenyl sulfone, 3 parts of 4,4'-difluorobenzophenone, 2 parts of 3,4'-difluorobenzophenone, 3 parts of 3-fluoro-4'-chlorobenzophenone, 120 parts of sulfone, 1 part of potassium bicarbonate, and 1 part of sodium carbonate. Combine the following ingredients: 4,4'-dihydroxydiphenyl sulfone, 4,4'-dichlorodiphenyl sulfone, 4,4'-difluorobenzophenone, 3,4'-difluorobenzophenone, and 3-fluoro-4'-chlorodiphenyl sulfone. Methyl ketone and sulfone were placed in a reactor equipped with a nitrogen purging pipe, a condenser, and a stirrer. The mixture was stirred and dissolved. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 200°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 260°C and kept at that temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained.
[0152] 2) Mix the polymer powder with acetone at a mass ratio of 1:20, boil for 3 hours, repeat this treatment 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
[0153] Preferably, the pressure in step (6) is 20 MPa and the temperature is 300 °C.
[0154] Test methods: Examples 1-3 and Comparative Examples 1-3 were compared, and comparative tests were conducted according to the national standard CB / T2410-2008 "Determination of Light Transmittance and Haze of Transparent Plastics" and GB / T1043.1-2008 "Determination of Impact Performance of Simply Supported Beams of Plastics". Specific test results are shown in Table 1.
[0155]
[0156]
[0157] A comparison of Examples 1-3 and Comparative Examples 1-3 in Table 1 shows that, by adding self-made polycarbonate, the present invention first introduces p-fluorobenzoyl chloride into 4-methoxy-4'-hydroxyazobenzene through a reaction to obtain a modifier. During the mixing process with polycarbonate, the carbon-oxygen double bonds in the modifier can undergo dipole-dipole interactions with the carbon-oxygen double bonds in polycarbonate, thereby weakening the interactions of the polycarbonate molecular chains, improving the flowability of the product, and enhancing the fluidity of the components in the system. This allows the components in the system to be fully mixed, thereby improving the mechanical properties and transparency of the product. At the same time, due to the addition of the modifier, the inter-chain spacing between the modifier and polycarbonate is reduced, which inhibits the crack propagation of the local segments of the polycarbonate molecular chains during the tensile process, causing the crack direction to be obstructed and shifted to the side, enhancing energy dissipation, and thus enhancing the tensile strength of the product. The present invention, by adding self-made polycarbonate... In resin production, firstly, since unmodified polyarylether sulfone is an amorphous polymer, its molecular chains are entangled. Due to the rigid structure of its molecular chains, the entanglement between rigid chains is not easily resolved, making the movement of the entire macromolecular chain difficult, resulting in a high melting temperature and decreased fluidity. After introducing ketone groups, since the ketone groups in the molecular chains are coplanar with the benzene rings, there is a certain interaction force between the molecular chains, which can break the entanglement between the polyarylether sulfone molecular chains. Moreover, since the content of ketone groups in the molecular chains is small, the π bond force between the molecular chains is weak. At this time, the decrease in the entanglement between the polyarylether sulfone molecular chains plays a dominant role in the effect on the polymer fluidity, thus improving the polymer fluidity. This increases the fluidity of the system, allowing the various components in the system to be mixed more thoroughly, reducing the generation of bubbles. At the same time, the increased fluidity allows the components in the system to fill the mold better, avoiding the impact of defects and unevenness on the mold surface on the light transmittance of the resin product.
[0158] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
[0159] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.
Claims
1. A processing technology for a high-transparency resin, characterized in that, Includes the following steps: (1) Prepare the homemade resin mixture; (2) Add appropriate additives to the homemade resin mixture; (3) Place the high-transparency resin particles in a dryer for pretreatment to remove moisture and impurities; (4) The pretreated resin particles are placed into the hopper of the injection molding machine and heated and melted to make them into a molten state; (5) Select a mold suitable for the required grid resin product and ensure that the mold has good optical surface quality; (6) Inject the molten self-made resin mixture into the groove of the grid forming mold, apply appropriate pressure and temperature, so that the self-made resin mixture fully fills the mold cavity to form the product; (7) Cool the mold to allow the resin to cure quickly; (8) Open the mold and remove the molded high-transparency molded grid resin product; (9) Post-processing of the molded products, namely deburring, trimming edges and polishing; The preparation steps of the self-made resin mixture in step (1) are as follows: By weight, take 20-30 parts of polymethyl methacrylate, 10-20 parts of homemade polycarbonate, 5-8 parts of homemade resin, and 1-2 parts of magnesium bis(trifluoromethanesulfonyl)imide. Place the polymethyl methacrylate, homemade polycarbonate, homemade resin, and magnesium bis(trifluoromethanesulfonyl)imide in a mixer and mix for 10-20 minutes at a temperature of 200-300℃ and a speed of 50 rpm. Then, place the resulting blend in a flat vulcanizing machine and hot-press it at a temperature of 200-300℃ and a pressure of 10-20 MPa. After cooling and crushing, the homemade resin mixture is obtained. The specific preparation process of the self-made polycarbonate is as follows: 1) By weight, take 1-2 parts of 4-methoxy-4'-hydroxyazobenzene, 1-2 parts of triethylamine, 1-2 parts of p-fluorobenzoyl chloride, and 200-300 parts of tetrahydrofuran. Dissolve 4-methoxy-4'-hydroxyazobenzene and triethylamine in tetrahydrofuran under a salt-ice bath. Then, add p-fluorobenzoyl chloride dropwise to the solution. After the addition is complete, remove the water bath and react at room temperature for 24-48 hours. Remove the tetrahydrofuran by rotary evaporation to obtain the rotary evaporation product. Wash the rotary evaporation product with ethanol 5-8 times, and then wash it repeatedly with distilled water and filter it 5-8 times to obtain a filter cake. Then, recrystallize the filter cake with a mixed solution of acetone / ethanol at a volume ratio of 3:5 to obtain the modifier. 2) By weight, take 2-3 parts of modifier, 20-30 parts of polycarbonate and 2-3 parts of pentaerythritol stearate. Place the reaction product, polycarbonate and pentaerythritol stearate in an extruder and extrude and granulate at a temperature of 200-300℃ to obtain the self-made polycarbonate. The specific preparation process of the self-made resin is as follows: 1) By weight, take 5-10 parts of 4,4'-dihydroxydiphenyl sulfone, 2-3 parts of 4,4'-dichlorodiphenyl sulfone, 2-3 parts of 4,4'-difluorobenzophenone, 2-3 parts of 3,4'-difluorobenzophenone, 2-3 parts of 3-fluoro-4'-chlorobenzophenone, 100-120 parts of sulfone, 1-2 parts of potassium bicarbonate, and 1-2 parts of sodium carbonate. [The remaining text appears to be a fragmented and incomplete sentence.] Benzene, 3,4'-difluorobenzophenone, 3-fluoro-4'-chlorobenzophenone, and sulfone were placed in a reactor equipped with a nitrogen inlet, a condenser, and a stirrer. The mixture was stirred until dissolved. After all the monomers were dissolved, potassium bicarbonate was added to the reactor, and the temperature was raised to 180-200°C. The salt formation reaction began and lasted for about 1 hour. The water generated in the system was condensed and discharged through the condenser. After the salt formation was completed, the temperature was raised to 230-260°C and kept at this temperature for 2 hours. A certain amount of sodium carbonate was added, and the reaction was continued for 1 hour. The mixture was then cooled, pulverized, and polymer powder was obtained. 2) Mix the polymer powder with acetone at a mass ratio of 1:10-1:20, boil for 2-3 hours, repeat this treatment 8 times, then add deionized water and boil for 1 hour, repeating this process multiple times until the chloride ion content in the water is below 5 ppm. Then dry the treated polymer powder and the moisture content is below 0.5% by weight to obtain the self-made resin.
2. The processing technology for a high-transparency resin according to claim 1, characterized in that, The additives mentioned in step (2) include UV stabilizers and antistatic agents.
3. The processing technology for a high-transparency resin according to claim 1, characterized in that, The pressure in step (6) is 10-20 MPa; the temperature is 200-400℃.