CN115819747A - Flame-retardant polycarbonate prepolymer with intrinsic sulfonate and compound thereof - Google Patents
Flame-retardant polycarbonate prepolymer with intrinsic sulfonate and compound thereof Download PDFInfo
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- 239000004417 polycarbonate Substances 0.000 title claims abstract description 275
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 273
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 239000003063 flame retardant Substances 0.000 title claims abstract description 55
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 23
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 60
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 81
- 238000001514 detection method Methods 0.000 claims description 77
- 238000005070 sampling Methods 0.000 claims description 75
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 64
- 238000010438 heat treatment Methods 0.000 claims description 57
- 239000003795 chemical substances by application Substances 0.000 claims description 50
- 238000001125 extrusion Methods 0.000 claims description 45
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- 230000003179 granulation Effects 0.000 claims description 45
- 238000006068 polycondensation reaction Methods 0.000 claims description 42
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims description 41
- 238000003756 stirring Methods 0.000 claims description 35
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- 239000000463 material Substances 0.000 claims description 22
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
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- WGMBWDBRVAKMOO-UHFFFAOYSA-L disodium;4-[2-(4-oxidophenyl)propan-2-yl]phenolate Chemical compound [Na+].[Na+].C=1C=C([O-])C=CC=1C(C)(C)C1=CC=C([O-])C=C1 WGMBWDBRVAKMOO-UHFFFAOYSA-L 0.000 claims description 14
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Abstract
The invention relates to the technical field of engineering plastics, in particular to an essential sulfonate flame-retardant polycarbonate prepolymer and a composition thereof, and provides the following scheme aiming at the problem that the performance of a prepared polycarbonate composition is poor due to the fact that the influence of the essential flame-retardant sulfonate polycarbonate prepolymer on the mechanical performance is large in the existing polycarbonate prepolymer and composition technology thereof, wherein the scheme comprises the following raw materials in parts by weight: 40-75 parts of bisphenol A containing a sulfonate structure, 30-55 parts of 50% sodium hydroxide solution, 10-35 parts of a toughening agent and 5-25 parts of a flame retardant.
Description
Technical Field
The invention relates to the technical field of engineering plastics, in particular to an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof.
Background
Polycarbonate (abbreviated as PC in english), also called PC plastic, is a high molecular polymer containing carbonate groups in its molecular chain, and can be classified into various types such as aliphatic, aromatic, aliphatic-aromatic, and the like, according to the structure of the ester groups. The polycarbonate is a polyester of carbonic acid, the carbonic acid is not stable per se, but derivatives (such as phosgene, urea, carbonate and carbonate) of the carbonic acid have certain stability, and the polycarbonate is weak acid resistant, weak alkali resistant and neutral oil resistant, but not ultraviolet light resistant and strong alkali resistant. The polycarbonate is colorless and transparent, heat-resistant, impact-resistant and flame-retardant at BI level, and has good mechanical properties at common use temperature. Compared with polymethyl methacrylate, the polycarbonate has good impact resistance, high refractive index and good processability, and has UL94V-2 grade flame retardant property without additives. Polycarbonate is a transparent material, and has good mechanical property, flame retardant property and high temperature resistance. As one of five engineering plastics, polycarbonate is applied to a plurality of fields such as plates in the building industry, automobile parts, medical appliances, aerospace, electronic and electric appliances, optical lenses, optical disk base materials, LED illumination and the like, and has wide market prospect.
However, the existing polycarbonate prepolymer and compound technology thereof still have the problem that the influence of the intrinsic flame-retardant sulfonate polycarbonate prepolymer on the mechanical property is large, so that the prepared polycarbonate compound has poor performance, and therefore, an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof are provided for solving the problem.
Disclosure of Invention
The invention aims to solve the problems that the existing polycarbonate prepolymer and compound technology still has great influence of the intrinsic flame-retardant sulfonate polycarbonate prepolymer on the mechanical property, so that the prepared polycarbonate compound has poor performance and the like, and provides the intrinsic sulfonate flame-retardant polycarbonate prepolymer and the compound thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof comprise the following raw materials in parts by weight: 40-75 parts of bisphenol A containing a sulfonate structure, 30-55 parts of 50% sodium hydroxide solution, 10-35 parts of a toughening agent, 5-25 parts of a flame retardant, 1-10 parts of a cold resistant agent, 3-18 parts of an antioxidant, 10-30 parts of a catalyst, 20-40 parts of phosgene, 25-60 parts of dichloromethane, 10-30 parts of a hydrogen peroxide initiator, 5-25 parts of an anti-dripping agent and 3-20 parts of a lubricant;
preferably, the feed comprises the following raw materials in parts by weight: 40-70 parts of bisphenol A containing a sulfonate structure, 30-50 parts of 50% sodium hydroxide solution, 10-32 parts of a toughening agent, 5-23 parts of a flame retardant, 1-8 parts of a cold resistant agent, 3-17 parts of an antioxidant, 10-28 parts of a catalyst, 20-38 parts of phosgene, 25-45 parts of dichloromethane, 10-28 parts of a hydrogen peroxide initiator, 5-23 parts of an anti-dripping agent and 8-20 parts of a lubricant;
preferably, the feed comprises the following raw materials in parts by weight: 40-55 parts of bisphenol A containing a sulfonate structure, 30-43 parts of 50% sodium hydroxide solution, 10-26 parts of a toughening agent, 5-19 parts of a flame retardant, 1-7 parts of a cold resistant agent, 3-15 parts of an antioxidant, 13-28 parts of a catalyst, 20-35 parts of phosgene, 25-40 parts of dichloromethane, 10-23 parts of a hydrogen peroxide initiator, 10-23 parts of an anti-dripping agent and 9-20 parts of a lubricant;
the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: obtaining raw materials by professionals, and pretreating the obtained raw materials by the professionals to prepare a polycarbonate prepolymer;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on the prepared polycarbonate prepolymer by professional personnel to prepare high molecular polycarbonate solution, and carrying out final treatment on the obtained powdery high molecular polycarbonate by the professional personnel to prepare a polycarbonate compound;
s3: and (3) real-time temperature detection: real-time temperature detection is carried out on a part of the process of preparing the polycarbonate compound by a professional;
s4: and (3) subsequent treatment: carrying out subsequent treatment by professional personnel;
preferably, in S1, a professional obtains a raw material, wherein the raw material includes bisphenol a containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, dichloromethane, a hydrogen peroxide initiator, an anti-dripping agent, and a lubricant, and the professional pretreats the obtained raw material to prepare a polycarbonate prepolymer, wherein the pretreatment is to select bisphenol a by the professional to perform a phosgene interfacial polycondensation process, and when the phosgene interfacial polycondensation process is performed, the professional reacts bisphenol a with the 50% sodium hydroxide solution to obtain a bisphenol a sodium salt, and sends the obtained bisphenol a sodium salt into a phosgenation reactor, dichloromethane is pre-provided in the phosgenation reactor as a solvent and a hydrogen peroxide initiator, and the presence ratio of the dichloromethane to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out a primary polymerization reaction to generate a polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min;
preferably, in S2, a professional performs a polycondensation reaction on the prepared polycarbonate prepolymer to prepare a high molecular polycarbonate solution, wherein a catalyst feed port is opened by the professional during the polycondensation reaction, the polycondensation reaction time is 20min, the catalyst is triethylamine, the prepared high molecular polycarbonate solution is purified by the professional after the polycondensation reaction is completed, a vapor deposition method is adopted during the purification, the vapor deposition method is to concentrate the prepared high molecular polycarbonate solution by the professional first, spray the concentrated high molecular polycarbonate solution into powder by using water vapor, evaporate and deposit a powdery high molecular polycarbonate by using an organic solvent, and perform final treatment on the obtained powdery high molecular polycarbonate by the professional to prepare a polycarbonate compound, wherein the professional mixes the obtained high molecular polycarbonate with other raw materials to obtain a polycarbonate compound raw material, wherein the professional weighs the polycarbonate compound raw material according to a material mixing ratio before the final treatment, and the material mixing ratio is high molecular polycarbonate: a toughening agent: flame retardant: cold-resistant agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, intensively collecting the raw materials of the polycarbonate compound, and sending the intensively collected raw materials of the polycarbonate compound into an extruder through a conveyor belt for extrusion granulation to obtain the polycarbonate compound, wherein the extruder needs to be preheated by the professional before the raw materials of the polycarbonate compound are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, the feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept between 300 and 400 ℃ during extrusion granulation;
preferably, in S3, a professional performs real-time temperature detection on a partial process of the preparation of the polycarbonate compound, wherein the partial process includes a preheating process and an extrusion granulation process, when performing real-time temperature detection, the professional turns on a switch of an infrared temperature detector, transmits infrared light to the interior of the extruder through the infrared temperature detector to obtain real-time temperature data of the interior of the extruder, displays the temperature data in real time through a temperature data display screen of the infrared temperature detector, observes the temperature data display screen in real time through the professional, performs judgment through a real-time observation result, processes the judgment result, wherein the real-time observation result shows that the temperature data display screen data exceeds 400 ℃, the preheating is judged to be completed, and the real-time observation result shows that the temperature data display screen data does not exceed 400 ℃, the preheating is judged to be incomplete, and the judging result is that the heating power of the heating device of the extruding machine is fixed when the preheating is finished, the feeding hole of the extruding machine is opened by a professional, the preheating is continued when the preheating is not finished, the heating power is increased by setting the heating device of the extruding machine by the professional when the preheating is continued, meanwhile, the temperature data display screen is observed in real time by the professional, the judgment is carried out according to the real-time observation result, the judgment result is processed until the preheating is finished and the heating power of the heating device of the extruding machine is fixed, the feeding hole of the extruding machine is opened by the professional, the extruding and granulating temperature is detected in real time by an infrared temperature detector after the preheating is finished, the extruding and granulating temperature is observed in real time by the professional through the temperature data display screen, and the judgment is carried out according to the observation result, processing through a judgment result, wherein the observation result shows that the temperature of the extrusion granulation process is normal when being within the range of 300-400 ℃, the observation result shows that the temperature of the extrusion granulation process is abnormal when not within the range of 300-400 ℃, the processing is not performed when the judgment result is normal, and the professional turns off the switch of the extruder switch when the judgment result is abnormal, and simultaneously calls a manager for processing;
preferably, in S4, a professional performs subsequent processing, wherein the professional puts the polycarbonate composite into an oven to perform a primary drying process when performing the subsequent processing, the oven temperature is kept at 100-110 ℃ during the primary drying process, the primary drying process lasts for 2 hours, and the professional performs sampling detection on the polycarbonate composite after the primary drying process is completed, wherein the sampling volume is as follows: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
Compared with the prior art, the invention has the beneficial effects that:
1. the polycarbonate prepolymer is prepared by adopting a phosgene interfacial polycondensation process, so that the reaction time is short, the byproducts are few, and the preparation success rate of the polycarbonate compound is improved.
2. By changing the raw materials of the formula, the influence of the inherent flame-retardant sulfonate polycarbonate prepolymer on the mechanical property is reduced, and the flame retardance and the impact toughness of the prepared polycarbonate compound are improved.
The invention aims to prepare polycarbonate prepolymer by adopting a phosgene interface polycondensation process, has short reaction time and few byproducts, improves the preparation success rate of polycarbonate compounds, reduces the influence of the intrinsic flame-retardant sulfonate polycarbonate prepolymer on the mechanical property by changing the raw materials of the formula, and improves the flame retardance and the impact toughness of the prepared polycarbonate compounds.
Drawings
FIG. 1 is a flow chart of a method for preparing an intrinsic sulfonate flame retardant polycarbonate prepolymer and a compound thereof according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
Referring to fig. 1, an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof comprise the following raw materials in parts by weight: 50 parts of bisphenol A containing a sulfonate structure, 36 parts of 50% sodium hydroxide solution, 18 parts of a toughening agent, 13 parts of a flame retardant, 5 parts of a cold resistant agent, 8 parts of an antioxidant, 20 parts of a catalyst, 27 parts of phosgene, 33 parts of dichloromethane, 16 parts of a hydrogen peroxide initiator, 16 parts of an anti-dripping agent and 14 parts of a lubricant;
the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: the method comprises the steps of obtaining raw materials by professionals, wherein the raw materials comprise bisphenol A containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, methylene dichloride, a hydrogen peroxide initiator, an anti-dripping agent and a lubricant, and the obtained raw materials are pretreated by the professionals to prepare a polycarbonate prepolymer, wherein the pretreatment is that the professionals select the bisphenol A to carry out phosgene interface polycondensation process, the professionals firstly carry out reaction on the bisphenol A and the 50% sodium hydroxide solution to obtain bisphenol A sodium salt when the phosgene interface polycondensation process is carried out, the professionals send the obtained bisphenol A sodium salt into a phosgenation reaction kettle, the phosgenation reaction kettle is pre-provided with the methylene dichloride as a solvent and the hydrogen peroxide initiator, and the existence ratio of the methylene dichloride to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out primary polymerization reaction to generate polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on a prepared polycarbonate prepolymer by a professional to prepare a high-molecular polycarbonate solution, wherein the professional opens a catalyst feeding hole during the polycondensation reaction, the polycondensation reaction time is 20min, triethylamine is used as the catalyst, the prepared high-molecular polycarbonate solution is purified by the professional after the polycondensation reaction is finished, a steam-out method is adopted during the purification, the steam-out method is that the professional firstly concentrates the prepared high-molecular polycarbonate solution, water vapor is sprayed into powder after the concentration, powdery high-molecular polycarbonate is separated out by evaporating an organic solvent, the professional finally treats the obtained powdery high-molecular polycarbonate to prepare a polycarbonate compound, the professional firstly mixes the obtained high-molecular polycarbonate with other raw materials to obtain a polycarbonate compound raw material during the final treatment, the professional weighs the polycarbonate compound raw material according to the material mixing ratio before the mixing, and the material mixing ratio is high-molecular polycarbonate: a toughening agent: flame retardant: cold-resistant agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, and stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, the polycarbonate compound raw materials are intensively collected, and the intensively collected polycarbonate compound raw materials are sent into an extruder by a conveyor belt for extrusion granulation to obtain a polycarbonate compound, wherein the extruder needs to be preheated by the professional before the polycarbonate compound raw materials are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, a feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept within the range of 300-400 ℃ during extrusion granulation;
s3: and (3) real-time temperature detection: the method comprises the steps of carrying out real-time temperature detection on partial processes of polycarbonate compound preparation by a professional, wherein the partial processes comprise a preheating process and an extrusion granulation process, when the real-time temperature detection is carried out, firstly, turning on a switch of an infrared temperature detector by the professional, emitting infrared rays to the interior of an extruder by the infrared temperature detector to obtain real-time temperature data in the extruder, displaying the temperature data in real time by a temperature data display screen of the infrared temperature detector, observing the temperature data display screen in real time by the professional, judging by real-time observation results, processing by judging results, wherein the real-time observation results show that the temperature data display screen data exceeds 400 ℃ and then judging as preheating is finished, the real-time observation results show that the temperature data display screen data does not exceed 400 ℃ and then judging as preheating is unfinished, and the judgment results show that the preheating is unfinished, fixing the heating power of the heating device of the extruder if the preheating is finished, opening a feed inlet by the professional, continuing to preheat, setting the heating power of the extruder by the professional, observing the temperature data display screen in real-time, processing results show that the preheating is finished by the professional, the heating device if the preheating is finished, the judgment results show that the heating of the extruder, the heating device, and the extruder is finished by the professional, and the judgment results show that the preheating is finished by the heating results show that the heating of the heating device if the professional, the preheating is finished, wherein the observation result shows that the temperature of the extrusion granulation process is within the range of 300-400 ℃ and then is judged to be normal, the observation result shows that the temperature of the extrusion granulation process is not within the range of 300-400 ℃ and then is judged to be abnormal, the judgment result is normal and then is not processed, and the judgment result is abnormal, and then a professional closes the switch of the extruder switch and calls a manager to process;
s4: and (3) subsequent treatment: carrying out subsequent treatment by a professional, wherein the professional puts the polycarbonate compound into an oven to carry out primary drying treatment when carrying out the subsequent treatment, the temperature of the oven is kept at 105 ℃ in the primary drying treatment process, the primary drying treatment time is 2h, the professional carries out sampling detection on the polycarbonate compound after the primary drying treatment is finished, and the sampling volume is as follows when the sampling detection is carried out: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
Example two
Referring to fig. 1, an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof comprise the following raw materials in parts by weight: 40 parts of bisphenol A containing a sulfonate structure, 30 parts of 50% sodium hydroxide solution, 10 parts of a toughening agent, 5 parts of a flame retardant, 1 part of a cold resistant agent, 3 parts of an antioxidant, 13 parts of a catalyst, 20 parts of phosgene, 25 parts of dichloromethane, 10 parts of a hydrogen peroxide initiator, 10 parts of an anti-dripping agent and 9 parts of a lubricant;
the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: the method comprises the steps of obtaining raw materials by professionals, wherein the raw materials comprise bisphenol A containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, methylene dichloride, a hydrogen peroxide initiator, an anti-dripping agent and a lubricant, and the acquired raw materials are pretreated by the professionals to prepare a polycarbonate prepolymer, wherein the pretreatment is that the professionals select the bisphenol A to carry out phosgene interface polycondensation process, the professionals firstly react the bisphenol A with the 50% sodium hydroxide solution to obtain bisphenol A sodium salt when the phosgene interface polycondensation process is carried out, the professionals send the obtained bisphenol A sodium salt into a phosgenation reaction kettle, the phosgenation reaction kettle is pre-provided with methylene dichloride as a solvent and the hydrogen peroxide initiator, and the existence ratio of the methylene dichloride to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out primary polymerization reaction to generate polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on a prepared polycarbonate prepolymer by a professional to prepare a high-molecular polycarbonate solution, wherein the professional opens a catalyst feeding hole during the polycondensation reaction, the polycondensation reaction time is 20min, triethylamine is used as the catalyst, the prepared high-molecular polycarbonate solution is purified by the professional after the polycondensation reaction is finished, a steam-out method is adopted during the purification, the steam-out method is that the professional firstly concentrates the prepared high-molecular polycarbonate solution, water vapor is sprayed into powder after the concentration, powdery high-molecular polycarbonate is separated out by evaporating an organic solvent, the professional finally treats the obtained powdery high-molecular polycarbonate to prepare a polycarbonate compound, the professional firstly mixes the obtained high-molecular polycarbonate with other raw materials to obtain a polycarbonate compound raw material during the final treatment, the professional weighs the polycarbonate compound raw material according to the material mixing ratio before the mixing, and the material mixing ratio is high-molecular polycarbonate: a toughening agent: flame retardant: cold resistance agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, and stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, the polycarbonate compound raw materials are intensively collected, and the intensively collected polycarbonate compound raw materials are sent into an extruder by a conveyor belt for extrusion granulation to obtain a polycarbonate compound, wherein the extruder needs to be preheated by the professional before the polycarbonate compound raw materials are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, a feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept within the range of 300-400 ℃ during extrusion granulation;
s3: and (3) real-time temperature detection: the method comprises the steps of carrying out real-time temperature detection on partial processes of polycarbonate compound preparation by a professional, wherein the partial processes comprise a preheating process and an extrusion granulation process, when the real-time temperature detection is carried out, firstly, turning on a switch of an infrared temperature detector by the professional, emitting infrared rays to the interior of an extruder by the infrared temperature detector to obtain real-time temperature data in the extruder, displaying the temperature data in real time by a temperature data display screen of the infrared temperature detector, observing the temperature data display screen in real time by the professional, judging by real-time observation results, processing by judging results, wherein the real-time observation results show that the temperature data display screen data exceeds 400 ℃ and then judging as preheating is finished, the real-time observation results show that the temperature data display screen data does not exceed 400 ℃ and then judging as preheating is unfinished, and the judgment results show that the preheating is unfinished, fixing the heating power of the heating device of the extruder if the preheating is finished, opening a feed inlet by the professional, continuing to preheat, setting the heating power of the extruder by the professional, observing the temperature data display screen in real-time, processing results show that the preheating is finished by the professional, the heating device if the preheating is finished, the judgment results show that the heating of the extruder, the heating device, and the extruder is finished by the professional, and the judgment results show that the preheating is finished by the heating results show that the heating of the heating device if the professional, the preheating is finished, wherein the observation result shows that the temperature of the extrusion granulation process is within the range of 300-400 ℃ and then is judged to be normal, the observation result shows that the temperature of the extrusion granulation process is not within the range of 300-400 ℃ and then is judged to be abnormal, the judgment result is normal and then is not processed, and the judgment result is abnormal, and then a professional closes the switch of the extruder switch and calls a manager to process;
s4: and (3) subsequent treatment: carrying out subsequent treatment by a professional, wherein the professional puts the polycarbonate compound into an oven for primary drying treatment when the subsequent treatment is carried out, the temperature of the oven is kept at 100 ℃ in the primary drying treatment process, the primary drying treatment time is 2h, the professional carries out sampling detection on the polycarbonate compound after the primary drying treatment is finished, and the sampling volume when the sampling detection is carried out is as follows: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
EXAMPLE III
Referring to fig. 1, an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof comprise the following raw materials in parts by weight: 55 parts of bisphenol A containing a sulfonate structure, 43 parts of 50% sodium hydroxide solution, 26 parts of a toughening agent, 19 parts of a flame retardant, 7 parts of a cold resistant agent, 15 parts of an antioxidant, 28 parts of a catalyst, 35 parts of phosgene, 40 parts of dichloromethane, 23 parts of a hydrogen peroxide initiator, 23 parts of an anti-dripping agent and 20 parts of a lubricant;
the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: the method comprises the steps of obtaining raw materials by professionals, wherein the raw materials comprise bisphenol A containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, methylene dichloride, a hydrogen peroxide initiator, an anti-dripping agent and a lubricant, and the obtained raw materials are pretreated by the professionals to prepare a polycarbonate prepolymer, wherein the pretreatment is that the professionals select the bisphenol A to carry out phosgene interface polycondensation process, the professionals firstly carry out reaction on the bisphenol A and the 50% sodium hydroxide solution to obtain bisphenol A sodium salt when the phosgene interface polycondensation process is carried out, the professionals send the obtained bisphenol A sodium salt into a phosgenation reaction kettle, the phosgenation reaction kettle is pre-provided with the methylene dichloride as a solvent and the hydrogen peroxide initiator, and the existence ratio of the methylene dichloride to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out primary polymerization reaction to generate polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on a prepared polycarbonate prepolymer by a professional to prepare a high-molecular polycarbonate solution, wherein the professional opens a catalyst feeding hole during the polycondensation reaction, the polycondensation reaction time is 20min, triethylamine is used as the catalyst, the prepared high-molecular polycarbonate solution is purified by the professional after the polycondensation reaction is finished, a steam-out method is adopted during the purification, the steam-out method is that the professional firstly concentrates the prepared high-molecular polycarbonate solution, water vapor is sprayed into powder after the concentration, powdery high-molecular polycarbonate is separated out by evaporating an organic solvent, the professional finally treats the obtained powdery high-molecular polycarbonate to prepare a polycarbonate compound, the professional firstly mixes the obtained high-molecular polycarbonate with other raw materials to obtain a polycarbonate compound raw material during the final treatment, the professional weighs the polycarbonate compound raw material according to the material mixing ratio before the mixing, and the material mixing ratio is high-molecular polycarbonate: a toughening agent: flame retardant: cold resistance agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, and stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, the polycarbonate compound raw materials are intensively collected, and the intensively collected polycarbonate compound raw materials are sent into an extruder by a conveyor belt for extrusion granulation to obtain a polycarbonate compound, wherein the extruder needs to be preheated by the professional before the polycarbonate compound raw materials are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, a feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept within the range of 300-400 ℃ during extrusion granulation;
s3: and (3) real-time temperature detection: the method comprises the steps of carrying out real-time temperature detection on partial processes of polycarbonate compound preparation by a professional, wherein the partial processes comprise a preheating process and an extrusion granulation process, when the real-time temperature detection is carried out, firstly, turning on a switch of an infrared temperature detector by the professional, emitting infrared rays to the interior of an extruder by the infrared temperature detector to obtain real-time temperature data in the extruder, displaying the temperature data in real time by a temperature data display screen of the infrared temperature detector, observing the temperature data display screen in real time by the professional, judging by real-time observation results, processing by judging results, wherein the real-time observation results show that the temperature data display screen data exceeds 400 ℃ and then judging as preheating is finished, the real-time observation results show that the temperature data display screen data does not exceed 400 ℃ and then judging as preheating is unfinished, and the judgment results show that the preheating is unfinished, fixing the heating power of the heating device of the extruder if the preheating is finished, opening a feed inlet by the professional, continuing to preheat, setting the heating power of the extruder by the professional, observing the temperature data display screen in real-time, processing results show that the preheating is finished by the professional, the heating device if the preheating is finished, the judgment results show that the heating of the extruder, the heating device, and the extruder is finished by the professional, and the judgment results show that the preheating is finished by the heating results show that the heating of the heating device if the professional, the preheating is finished, wherein the observation result shows that the temperature of the extrusion granulation process is within the range of 300-400 ℃ and then is judged to be normal, the observation result shows that the temperature of the extrusion granulation process is not within the range of 300-400 ℃ and then is judged to be abnormal, the judgment result is normal and then is not processed, and the judgment result is abnormal, and then a professional closes the switch of the extruder switch and calls a manager to process;
s4: and (3) subsequent treatment: carrying out subsequent treatment by a professional, wherein the professional puts the polycarbonate compound into an oven to carry out primary drying treatment when carrying out the subsequent treatment, the temperature of the oven is kept at 110 ℃ in the primary drying treatment process, the primary drying treatment time is 2h, the professional carries out sampling detection on the polycarbonate compound after the primary drying treatment is finished, and the sampling volume is as follows when the sampling detection is carried out: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
Example four
Referring to fig. 1, an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof comprise the following raw materials in parts by weight: 55 parts of bisphenol A containing a sulfonate structure, 30 parts of 50% sodium hydroxide solution, 26 parts of a toughening agent, 5 parts of a flame retardant, 7 parts of a cold resistant agent, 3 parts of an antioxidant, 28 parts of a catalyst, 20 parts of phosgene, 40 parts of dichloromethane, 10 parts of a hydrogen peroxide initiator, 23 parts of an anti-dripping agent and 9 parts of a lubricant;
the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: the method comprises the steps of obtaining raw materials by professionals, wherein the raw materials comprise bisphenol A containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, methylene dichloride, a hydrogen peroxide initiator, an anti-dripping agent and a lubricant, and the obtained raw materials are pretreated by the professionals to prepare a polycarbonate prepolymer, wherein the pretreatment is that the professionals select the bisphenol A to carry out phosgene interface polycondensation process, the professionals firstly carry out reaction on the bisphenol A and the 50% sodium hydroxide solution to obtain bisphenol A sodium salt when the phosgene interface polycondensation process is carried out, the professionals send the obtained bisphenol A sodium salt into a phosgenation reaction kettle, the phosgenation reaction kettle is pre-provided with the methylene dichloride as a solvent and the hydrogen peroxide initiator, and the existence ratio of the methylene dichloride to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out primary polymerization reaction to generate polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on a prepared polycarbonate prepolymer by a professional to prepare a high-molecular polycarbonate solution, wherein the professional opens a catalyst feeding hole during the polycondensation reaction, the polycondensation reaction time is 20min, triethylamine is used as the catalyst, the prepared high-molecular polycarbonate solution is purified by the professional after the polycondensation reaction is finished, a steam-out method is adopted during the purification, the steam-out method is that the professional firstly concentrates the prepared high-molecular polycarbonate solution, water vapor is sprayed into powder after the concentration, powdery high-molecular polycarbonate is separated out by evaporating an organic solvent, the professional finally treats the obtained powdery high-molecular polycarbonate to prepare a polycarbonate compound, the professional firstly mixes the obtained high-molecular polycarbonate with other raw materials to obtain a polycarbonate compound raw material during the final treatment, the professional weighs the polycarbonate compound raw material according to the material mixing ratio before the mixing, and the material mixing ratio is high-molecular polycarbonate: a toughening agent: flame retardant: cold resistance agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, and stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, the polycarbonate compound raw materials are intensively collected, and the intensively collected polycarbonate compound raw materials are sent into an extruder by a conveyor belt for extrusion granulation to obtain a polycarbonate compound, wherein the extruder needs to be preheated by the professional before the polycarbonate compound raw materials are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, a feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept within the range of 300-400 ℃ during extrusion granulation;
s3: and (3) real-time temperature detection: the method comprises the steps of carrying out real-time temperature detection on partial processes of polycarbonate compound preparation by a professional, wherein the partial processes comprise a preheating process and an extrusion granulation process, when the real-time temperature detection is carried out, firstly, turning on a switch of an infrared temperature detector by the professional, emitting infrared rays to the interior of an extruder by the infrared temperature detector to obtain real-time temperature data in the extruder, displaying the temperature data in real time by a temperature data display screen of the infrared temperature detector, observing the temperature data display screen in real time by the professional, judging by real-time observation results, processing by judging results, wherein the real-time observation results show that the temperature data display screen data exceeds 400 ℃ and then judging as preheating is finished, the real-time observation results show that the temperature data display screen data does not exceed 400 ℃ and then judging as preheating is unfinished, and the judgment results show that the preheating is unfinished, fixing the heating power of the heating device of the extruder if the preheating is finished, opening a feed inlet by the professional, continuing to preheat, setting the heating power of the extruder by the professional, observing the temperature data display screen in real-time, processing results show that the preheating is finished by the professional, the heating device if the preheating is finished, the judgment results show that the heating of the extruder, the heating device, and the extruder is finished by the professional, and the judgment results show that the preheating is finished by the heating results show that the heating of the heating device if the professional, the preheating is finished, wherein the observation result shows that the temperature of the extrusion granulation process is within the range of 300-400 ℃ and then is judged to be normal, the observation result shows that the temperature of the extrusion granulation process is not within the range of 300-400 ℃ and then is judged to be abnormal, the judgment result is normal and then is not processed, and the judgment result is abnormal, and then a professional closes the switch of the extruder switch and calls a manager to process;
s4: and (3) subsequent treatment: carrying out subsequent treatment by a professional, wherein the professional puts the polycarbonate compound into an oven to carry out primary drying treatment when carrying out the subsequent treatment, the temperature of the oven is kept at 103 ℃ in the primary drying treatment process, the primary drying treatment time is 2h, the professional carries out sampling detection on the polycarbonate compound after the primary drying treatment is finished, and the sampling volume is as follows when the sampling detection is carried out: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
EXAMPLE five
Referring to fig. 1, an intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof comprise the following raw materials in parts by weight: 44 parts of bisphenol A containing a sulfonate structure, 32 parts of 50% sodium hydroxide solution, 15 parts of a toughening agent, 7 parts of a flame retardant, 6 parts of a cold resistant agent, 11 parts of an antioxidant, 19 parts of a catalyst, 26 parts of phosgene, 30 parts of dichloromethane, 13 parts of a hydrogen peroxide initiator, 18 parts of an anti-dripping agent and 10 parts of a lubricant;
the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: the method comprises the steps of obtaining raw materials by professionals, wherein the raw materials comprise bisphenol A containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, methylene dichloride, a hydrogen peroxide initiator, an anti-dripping agent and a lubricant, and the obtained raw materials are pretreated by the professionals to prepare a polycarbonate prepolymer, wherein the pretreatment is that the professionals select the bisphenol A to carry out phosgene interface polycondensation process, the professionals firstly carry out reaction on the bisphenol A and the 50% sodium hydroxide solution to obtain bisphenol A sodium salt when the phosgene interface polycondensation process is carried out, the professionals send the obtained bisphenol A sodium salt into a phosgenation reaction kettle, the phosgenation reaction kettle is pre-provided with the methylene dichloride as a solvent and the hydrogen peroxide initiator, and the existence ratio of the methylene dichloride to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out primary polymerization reaction to generate polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on the prepared polycarbonate prepolymer by a professional to prepare a high-molecular polycarbonate solution, wherein the professional opens a catalyst inlet during the polycondensation reaction, the polycondensation reaction time is 20min, triethylamine is used as the catalyst, the prepared high-molecular polycarbonate solution is purified by the professional after the polycondensation reaction is finished, a steam-out method is adopted during the purification, the steam-out method is characterized in that the prepared high-molecular polycarbonate solution is firstly concentrated by the professional, water vapor is sprayed into powder after the concentration, the obtained powdery high-molecular polycarbonate is evaporated and separated out by an organic solvent, the acquired powdery high-molecular polycarbonate is finally processed by the professional to prepare a polycarbonate compound, the acquired high-molecular polycarbonate is firstly mixed with other raw materials by the professional during the final processing to obtain a polycarbonate compound raw material, the professional weighs the polycarbonate compound according to the material mixing ratio before the mixing, and the material mixing ratio is the high-molecular polycarbonate: a toughening agent: flame retardant: cold resistance agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, and stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, the polycarbonate compound raw materials are intensively collected, and the intensively collected polycarbonate compound raw materials are sent into an extruder by a conveyor belt for extrusion granulation to obtain a polycarbonate compound, wherein the extruder needs to be preheated by the professional before the polycarbonate compound raw materials are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, a feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept within the range of 300-400 ℃ during extrusion granulation;
s3: and (3) real-time temperature detection: the method comprises the steps of carrying out real-time temperature detection on partial processes of polycarbonate compound preparation by a professional, wherein the partial processes comprise a preheating process and an extrusion granulation process, when the real-time temperature detection is carried out, firstly, turning on a switch of an infrared temperature detector by the professional, emitting infrared rays to the interior of an extruder by the infrared temperature detector to obtain real-time temperature data in the extruder, displaying the temperature data in real time by a temperature data display screen of the infrared temperature detector, observing the temperature data display screen in real time by the professional, judging by real-time observation results, processing by judging results, wherein the real-time observation results show that the temperature data display screen data exceeds 400 ℃ and then judging as preheating is finished, the real-time observation results show that the temperature data display screen data does not exceed 400 ℃ and then judging as preheating is unfinished, and the judgment results show that the preheating is unfinished, fixing the heating power of the heating device of the extruder if the preheating is finished, opening a feed inlet by the professional, continuing to preheat, setting the heating power of the extruder by the professional, observing the temperature data display screen in real-time, processing results show that the preheating is finished by the professional, the heating device if the preheating is finished, the judgment results show that the heating of the extruder, the heating device, and the extruder is finished by the professional, and the judgment results show that the preheating is finished by the heating results show that the heating of the heating device if the professional, the preheating is finished, wherein the observation result shows that the temperature of the extrusion granulation process is within the range of 300-400 ℃ and then is judged to be normal, the observation result shows that the temperature of the extrusion granulation process is not within the range of 300-400 ℃ and then is judged to be abnormal, the judgment result is normal and then is not processed, and the judgment result is abnormal, and then a professional closes the switch of the extruder switch and calls a manager to process;
s4: and (3) subsequent treatment: carrying out subsequent treatment by a professional, wherein the professional puts the polycarbonate compound into an oven to carry out primary drying treatment when carrying out the subsequent treatment, the temperature of the oven is kept at 101 ℃ in the primary drying treatment process, the primary drying treatment time is 2h, the professional carries out sampling detection on the polycarbonate compound after the primary drying treatment is finished, and the sampling volume is as follows when the sampling detection is carried out: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
An intrinsic sulfonate flame retardant polycarbonate prepolymer and a compound thereof in the first, second, third, fourth and fifth examples were tested, and the following results were obtained:
the preparation success rate and the product performance of the intrinsic sulfonate flame-retardant polycarbonate prepolymer and the compound thereof prepared in the first embodiment, the second embodiment, the third embodiment, the fourth embodiment and the fifth embodiment are obviously improved compared with the existing polycarbonate prepolymer and the compound thereof, and the first embodiment is the best embodiment.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. An intrinsic sulfonate flame-retardant polycarbonate prepolymer and a compound thereof are characterized by comprising the following raw materials in parts by weight: 40-75 parts of bisphenol A containing a sulfonate structure, 30-55 parts of 50% sodium hydroxide solution, 10-35 parts of a toughening agent, 5-25 parts of a flame retardant, 1-10 parts of a cold resistant agent, 3-18 parts of an antioxidant, 10-30 parts of a catalyst, 20-40 parts of phosgene, 25-60 parts of dichloromethane, 10-30 parts of a hydrogen peroxide initiator, 5-25 parts of an anti-dripping agent and 3-20 parts of a lubricant.
2. The polycarbonate prepolymer and the polycarbonate composition containing the same as described in claim 1, wherein the polycarbonate prepolymer comprises the following raw materials in parts by weight: 40-70 parts of bisphenol A containing a sulfonate structure, 30-50 parts of 50% sodium hydroxide solution, 10-32 parts of a toughening agent, 5-23 parts of a flame retardant, 1-8 parts of a cold resistant agent, 3-17 parts of an antioxidant, 10-28 parts of a catalyst, 20-38 parts of phosgene, 25-45 parts of dichloromethane, 10-28 parts of a hydrogen peroxide initiator, 5-23 parts of an anti-dripping agent and 8-20 parts of a lubricant.
3. The flame retardant polycarbonate prepolymer of claim 1, which is prepared from the following raw materials in parts by weight: 40-55 parts of bisphenol A containing a sulfonate structure, 30-43 parts of 50% sodium hydroxide solution, 10-26 parts of a toughening agent, 5-19 parts of a flame retardant, 1-7 parts of a cold resistant agent, 3-15 parts of an antioxidant, 13-28 parts of a catalyst, 20-35 parts of phosgene, 25-40 parts of dichloromethane, 10-23 parts of a hydrogen peroxide initiator, 10-23 parts of an anti-dripping agent and 9-20 parts of a lubricant.
4. The flame retardant polycarbonate prepolymer of claim 1, wherein the preparation method comprises the following steps:
s1: preparation of polycarbonate prepolymer: obtaining raw materials by professionals, and pretreating the obtained raw materials by the professionals to prepare a polycarbonate prepolymer;
s2: preparation of polycarbonate composites: carrying out polycondensation reaction on the prepared polycarbonate prepolymer by professional personnel to prepare high molecular polycarbonate solution, and carrying out final treatment on the obtained powdery high molecular polycarbonate by the professional personnel to prepare a polycarbonate compound;
s3: and (3) real-time temperature detection: real-time temperature detection is carried out on a part of the process of preparing the polycarbonate compound by a professional;
s4: and (3) post-treatment: the subsequent treatment is carried out by a professional.
5. The intrinsic sulfonate flame retardant polycarbonate prepolymer and the compound thereof according to claim 4, wherein in the step S1, raw materials are obtained by professionals, wherein the raw materials comprise bisphenol A containing a sulfonate structure, a 50% sodium hydroxide solution, a toughening agent, a flame retardant, a cold resistant agent, an antioxidant, a catalyst, phosgene, dichloromethane, a hydrogen peroxide initiator, an anti-dripping agent and a lubricant, and the obtained raw materials are pretreated by the professionals to prepare the polycarbonate prepolymer, wherein the pretreatment is that the professional selects bisphenol A to carry out a phosgene interface polycondensation process, the professional firstly carries out a reaction between the bisphenol A and the 50% sodium hydroxide solution to obtain a bisphenol A sodium salt, and the professional sends the obtained bisphenol A sodium salt into a phosgenation reaction kettle, wherein dichloromethane is preset in the phosgenation reaction kettle as a solvent and the hydrogen peroxide initiator, and the existence ratio of the dichloromethane to the hydrogen peroxide initiator is 4: simultaneously introducing phosgene by professionals to carry out primary polymerization reaction to generate polycarbonate prepolymer, wherein the primary polymerization reaction time is 10min.
6. The intrinsic sulfonate flame retardant polycarbonate prepolymer and the composition thereof as claimed in claim 4, wherein in step S2, a professional performs a polycondensation reaction on the prepared polycarbonate prepolymer to prepare a high molecular polycarbonate solution, wherein the professional opens a catalyst inlet during the polycondensation reaction, the polycondensation reaction lasts for 20min, and triethylamine is used as the catalyst, after the polycondensation reaction is completed, the prepared high molecular polycarbonate solution is purified by the professional, wherein a vapor deposition method is used during the purification, the vapor deposition method is that the professional first concentrates the prepared high molecular polycarbonate solution, and sprays water vapor into powder, the powdered high molecular polycarbonate is separated by evaporating an organic solvent, and the professional performs a final treatment on the obtained powdered high molecular polycarbonate to prepare the polycarbonate composition, wherein the professional performs a final treatment on the obtained powdered high molecular polycarbonate and other raw materials to obtain polycarbonate composition raw materials, wherein the professional performs a weighing according to a material mixing ratio before the mixing, and the material mixing ratio is that the high molecular polycarbonate: a toughening agent: flame retardant: cold resistance agent: antioxidant: anti-dripping agent: the volume ratio of the lubricant used is 5:4:3:2:2:1:1, after weighing, putting weighed materials into a stirrer by a professional, stirring by the stirrer, wherein the stirring speed of the stirrer is 120r/min during stirring, the stirring time is 40min, after stirring, intensively collecting the raw materials of the polycarbonate compound, and sending the intensively collected raw materials of the polycarbonate compound into an extruder by a conveyor belt for extrusion granulation to obtain the polycarbonate compound, wherein the extruder needs to be preheated by the professional before the raw materials of the polycarbonate compound are sent into the extruder, after preheating, the professional sets the operation data of the extruder, and simultaneously, a feed inlet of the extruder is opened for extrusion granulation, and the temperature of the extruder is kept at 300-400 ℃ during extrusion granulation.
7. The polycarbonate prepolymer and the polycarbonate composition as claimed in claim 4, wherein in step S3, the professional carries out real-time temperature detection on the partial polycarbonate composition preparation process, wherein the partial process comprises a preheating process and an extrusion granulation process, when the real-time temperature detection is carried out, the professional turns on an infrared temperature detector switch, the infrared temperature detector emits infrared light to the interior of the extruder to obtain real-time temperature data inside the extruder, the temperature data is displayed on a temperature data display screen of the infrared temperature detector in real time, the professional carries out real-time observation on the temperature data display screen, the real-time observation result is used for judgment, the judgment result is carried out, and the real-time observation result shows that the temperature data display screen data exceeds 400 ℃, the preheating is judged to be completed, real-time observation results show that the data of a temperature data display screen does not exceed 400 ℃, the preheating is judged to be incomplete, the heating power of a heating device of the extruder is fixed if the preheating is completed, a professional opens a feed port of the extruder, the preheating is continued if the preheating is incomplete, the professional needs to set the heating device of the extruder to increase the heating power when the preheating is continued, the professional observes the temperature data display screen in real time, the judgment is carried out according to the real-time observation results, the judgment is carried out according to the judgment results, the heating power of the heating device of the extruder is fixed until the preheating is completed, the professional opens the feed port of the extruder, and the infrared temperature detector detects the extrusion granulation temperature in real time after the preheating is completed, and a professional observes the extrusion granulation temperature in real time through a temperature data display screen, judges the temperature through an observation result, and processes the temperature through a judgment result, wherein the observation result shows that the temperature of the extrusion granulation process is normal when the temperature is within the range of 300-400 ℃, the observation result shows that the temperature of the extrusion granulation process is abnormal when the temperature is not within the range of 300-400 ℃, the temperature is not normal when the temperature is abnormal, the extrusion granulation process is not processed when the temperature is normal, the professional closes an electric switch of an extruder when the temperature is abnormal, and meanwhile, a manager is called to process the temperature.
8. The flame retardant polycarbonate prepolymer of claim 4, wherein in the step S4, the professional carries out the subsequent treatment, wherein the professional puts the polycarbonate compound into the oven to carry out the primary drying treatment in the subsequent treatment, the temperature of the oven is kept between 100 and 110 ℃ in the primary drying treatment, the primary drying treatment lasts for 2 hours, the professional carries out the sampling detection on the polycarbonate compound after the primary drying treatment is finished, and the sampling volume is as follows: the total volume of the polycarbonate compound is 1:199, judging by sampling detection results, processing by judgment results, wherein the sampling results show that the water content of the polycarbonate compound exceeds 0.02%, judging that the drying treatment is unsuccessful, the sampling results show that the water content of the polycarbonate compound does not exceed 0.02%, judging that the drying treatment is successful, and judging that the drying treatment is unsuccessful, performing secondary drying treatment, wherein the conditions of the secondary drying treatment and the primary drying treatment are the same, performing sampling detection on the polycarbonate compound after the secondary drying treatment is completed by professionals, judging and processing by the sampling detection results, stopping the sampling detection until the drying treatment is successful, stopping the sampling detection if the judgment result is successful, and testing the sampled sample of the last sampling detection by the professionals, wherein the test contents comprise the flame retardancy, the tensile strength, the elongation at break and other performance data of the polycarbonate compound during the test, recording the performance data obtained by the professionals, comparing the obtained performance data with the performance data of the existing polycarbonate compound, judging that the performance data recorded during the test is superior to the performance data obtained by the professional, and calculating that the polycarbonate compound is prepared by the professional, and judging that the success rate is inferior to the polycarbonate compound.
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Citations (5)
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|---|---|---|---|---|
| US4403087A (en) * | 1981-09-28 | 1983-09-06 | General Electric Company | Polycarbonates chain terminated with sulfonic acid salt containing phenols |
| WO1984004312A1 (en) * | 1983-05-04 | 1984-11-08 | Gen Electric | Composition comprising flame retardant end-capped polycarbonate |
| CN107674399A (en) * | 2017-11-17 | 2018-02-09 | 成都双瑞暖通设备有限公司 | For preparing air-conditioner outdoor unit shell plastics |
| CN112898553A (en) * | 2021-01-25 | 2021-06-04 | 四川大学 | Efficient intrinsic flame-retardant polycarbonate and preparation method thereof |
| CN115028912A (en) * | 2022-06-06 | 2022-09-09 | 浙江六环电缆科技股份有限公司 | Low-smoke halogen-free low-toxicity flame-retardant polyolefin sheath material |
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2022
- 2022-11-04 CN CN202211375518.4A patent/CN115819747A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4403087A (en) * | 1981-09-28 | 1983-09-06 | General Electric Company | Polycarbonates chain terminated with sulfonic acid salt containing phenols |
| WO1984004312A1 (en) * | 1983-05-04 | 1984-11-08 | Gen Electric | Composition comprising flame retardant end-capped polycarbonate |
| CN107674399A (en) * | 2017-11-17 | 2018-02-09 | 成都双瑞暖通设备有限公司 | For preparing air-conditioner outdoor unit shell plastics |
| CN112898553A (en) * | 2021-01-25 | 2021-06-04 | 四川大学 | Efficient intrinsic flame-retardant polycarbonate and preparation method thereof |
| CN115028912A (en) * | 2022-06-06 | 2022-09-09 | 浙江六环电缆科技股份有限公司 | Low-smoke halogen-free low-toxicity flame-retardant polyolefin sheath material |
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