CN118459743A - A non-bisphenol A type medical polycarbonate and its preparation process - Google Patents
A non-bisphenol A type medical polycarbonate and its preparation process Download PDFInfo
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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 title claims abstract description 101
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 66
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 diphenol compound Chemical class 0.000 claims abstract description 45
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000000155 melt Substances 0.000 claims description 36
- 238000005809 transesterification reaction Methods 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000011541 reaction mixture Substances 0.000 claims description 14
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 14
- 239000007790 solid phase Substances 0.000 claims description 14
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 14
- 238000001125 extrusion Methods 0.000 claims description 12
- IJBWMYBRNPIXJT-UHFFFAOYSA-N 2,3-bis(2-phenylpropan-2-yl)phenol Chemical compound C=1C=CC(O)=C(C(C)(C)C=2C=CC=CC=2)C=1C(C)(C)C1=CC=CC=C1 IJBWMYBRNPIXJT-UHFFFAOYSA-N 0.000 claims description 7
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 claims description 7
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 7
- ROORDVPLFPIABK-UHFFFAOYSA-N diphenyl carbonate Chemical compound C=1C=CC=CC=1OC(=O)OC1=CC=CC=C1 ROORDVPLFPIABK-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- QBDSZLJBMIMQRS-UHFFFAOYSA-N p-Cumylphenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=CC=C1 QBDSZLJBMIMQRS-UHFFFAOYSA-N 0.000 claims description 7
- NKTOLZVEWDHZMU-UHFFFAOYSA-N p-cumyl phenol Natural products CC1=CC=C(C)C(O)=C1 NKTOLZVEWDHZMU-UHFFFAOYSA-N 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229940106691 bisphenol a Drugs 0.000 claims 12
- 239000000047 product Substances 0.000 claims 5
- 239000012043 crude product Substances 0.000 claims 2
- XKZQKPRCPNGNFR-UHFFFAOYSA-N 2-(3-hydroxyphenyl)phenol Chemical class OC1=CC=CC(C=2C(=CC=CC=2)O)=C1 XKZQKPRCPNGNFR-UHFFFAOYSA-N 0.000 claims 1
- 229930185605 Bisphenol Natural products 0.000 claims 1
- 239000002981 blocking agent Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000005453 pelletization Methods 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 6
- 239000002861 polymer material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/30—General preparatory processes using carbonates
- C08G64/307—General preparatory processes using carbonates and phenols
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
- Materials For Medical Uses (AREA)
Abstract
本发明公开了一种非双酚A型医用聚碳酸酯及其制备工艺，其中，一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：非双酚A型二酚化合物：50‑70wt％；碳酸二酯类化合物：20‑40wt％；封端剂：1‑5wt％；催化剂：0.01‑0.1wt％；本发明的非双酚A型医用聚碳酸酯具有优异的物理性能和化学稳定性，能够满足医疗领域对材料性能的高要求，同时，由于采用非双酚A型二酚化合物作为主链构建单元，避免了双酚A可能带来的健康风险，具有更高的安全性和环保性，更适合于医疗领域的应用，此外，本发明的制备方法流程简单、操作方便、成本低廉，具有较高的经济效益和社会效益。The invention discloses a non-bisphenol A type medical polycarbonate and a preparation process thereof. The non-bisphenol A type medical polycarbonate comprises the following components in percentage by mass: a non-bisphenol A type diphenol compound: 50-70wt%; a carbonic acid diester compound: 20-40wt%; a capping agent: 1-5wt%; and a catalyst: 0.01-0.1wt%. The non-bisphenol A type medical polycarbonate has excellent physical properties and chemical stability, and can meet the high requirements of the medical field for material properties. At the same time, since the non-bisphenol A type diphenol compound is used as a main chain building unit, the health risks that may be caused by bisphenol A are avoided, the polycarbonate has higher safety and environmental protection, and is more suitable for application in the medical field. In addition, the preparation method of the invention has a simple process, is easy to operate, is low in cost, and has higher economic and social benefits.
Description
技术领域Technical Field
本发明属于高分子材料技术领域，具体为一种非双酚A型医用聚碳酸酯及其制备工艺。The invention belongs to the technical field of polymer materials, and specifically relates to a non-bisphenol A type medical polycarbonate and a preparation process thereof.
背景技术Background Art
随着医疗技术的不断进步，对医用高分子材料的要求也越来越高。聚碳酸酯作为一种重要的高分子材料，因其优异的性能被广泛应用于医疗器械的制造中，在医疗领域具有广泛的应用。With the continuous advancement of medical technology, the requirements for medical polymer materials are getting higher and higher. Polycarbonate, as an important polymer material, is widely used in the manufacture of medical devices due to its excellent performance and has a wide range of applications in the medical field.
然而，传统的双酚A型聚碳酸酯因含有潜在的有害物质双酚A，其在医疗领域的应用受到一定的限制，因此，开发一种非双酚A型医用聚碳酸酯具有重要的实际意义。However, the application of traditional bisphenol A type polycarbonate in the medical field is limited to a certain extent because it contains the potentially harmful substance bisphenol A. Therefore, the development of a non-bisphenol A type medical polycarbonate has important practical significance.
发明内容Summary of the invention
针对上述情况，为克服现有技术的缺陷，本发明提供一种非双酚A型医用聚碳酸酯及其制备工艺，有效地解决了解决了上述背景提出的问题。In view of the above situation, in order to overcome the defects of the prior art, the present invention provides a non-bisphenol A medical polycarbonate and a preparation process thereof, which effectively solves the problems raised in the above background.
为实现上述目的，本发明提供如下技术方案：一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：To achieve the above object, the present invention provides the following technical solution: a non-bisphenol A medical polycarbonate, comprising the following components in percentage by mass:
非双酚A型二酚化合物：50-70wt％；Non-bisphenol A type diphenol compound: 50-70wt%;
碳酸二酯类化合物：20-40wt％；Carbonic acid diester compounds: 20-40wt%;
封端剂：1-5wt％；Capping agent: 1-5wt%;
催化剂：0.01-0.1wt％。Catalyst: 0.01-0.1wt%.
优选的，所述非双酚A型二酚化合物为对苯二酚、间苯二酚、联苯二酚中的一种。Preferably, the non-bisphenol A type diphenol compound is one of hydroquinone, resorcinol and biphenol.
优选的，所述碳酸二酯类化合物为碳酸二苯酯、碳酸二甲酯、碳酸二乙酯中的一种。Preferably, the carbonic acid diester compound is one of diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
优选的，所述封端剂为对枯基苯酚、二枯基苯酚、对叔丁基苯酚中的一种。Preferably, the end-capping agent is one of p-cumylphenol, dicumylphenol and p-tert-butylphenol.
优选的，所述催化剂为四丁基溴化铵、三苯基膦中的一种。Preferably, the catalyst is one of tetrabutylammonium bromide and triphenylphosphine.
一种非双酚A型医用聚碳酸酯的制备工艺，包括以下步骤：A preparation process of non-bisphenol A type medical polycarbonate comprises the following steps:
S1：将非双酚A型二酚化合物、碳酸二芳基酯、封端剂和催化剂按照上述成分比例混合均匀，得到反应混合物；S1: uniformly mixing a non-bisphenol A type diphenol compound, a diaryl carbonate, a capping agent and a catalyst according to the above-mentioned component ratio to obtain a reaction mixture;
S2：将反应混合物加入熔融酯交换反应器中，在氮气保护下进行熔融酯交换反应；S2: adding the reaction mixture into a melt transesterification reactor, and performing a melt transesterification reaction under nitrogen protection;
S3：将熔融酯交换反应后的产物进行固液分离，得到固相产物和液相产物。S3: performing solid-liquid separation on the product after the melt transesterification reaction to obtain a solid phase product and a liquid phase product.
S4：将固相产物进行真空干燥处理，得到干燥后的聚碳酸酯粗品；S4: vacuum drying the solid phase product to obtain a dried crude polycarbonate product;
S5：将干燥后的聚碳酸酯粗品进行熔融挤出处理，熔融挤出机的长径比为30-50:1，熔融温度为250-300℃，得到熔融挤出后的聚碳酸酯；S5: melt-extrude the dried crude polycarbonate, wherein the aspect ratio of the melt extruder is 30-50:1 and the melting temperature is 250-300° C. to obtain the polycarbonate after melt extrusion;
S6：将熔融挤出后的聚碳酸酯进行冷却切粒处理，得到最终的非双酚A型医用聚碳酸酯产品。S6: Cooling and pelletizing the melt-extruded polycarbonate to obtain a final non-bisphenol A medical polycarbonate product.
优选的，S2中，熔融酯交换反应，反应温度为200-250℃，反应时间为2-4h。Preferably, in S2, the melt transesterification reaction has a reaction temperature of 200-250° C. and a reaction time of 2-4 h.
优选的，S4中，干燥温度为100-120℃，干燥时间为2-4h。Preferably, in S4, the drying temperature is 100-120° C. and the drying time is 2-4 h.
与现有技术相比，本发明的有益效果是：Compared with the prior art, the present invention has the following beneficial effects:
本发明的非双酚A型医用聚碳酸酯具有优异的物理性能和化学稳定性，能够满足医疗领域对材料性能的高要求，同时，由于采用非双酚A型二酚化合物作为主链构建单元，避免了双酚A可能带来的健康风险，具有更高的安全性和环保性，更适合于医疗领域的应用，此外，本发明的制备方法流程简单、操作方便、成本低廉，具有较高的经济效益和社会效益。The non-bisphenol A type medical polycarbonate of the present invention has excellent physical properties and chemical stability, and can meet the high requirements of the medical field for material properties. At the same time, since the non-bisphenol A type diphenol compound is used as the main chain building unit, the health risks that may be caused by bisphenol A are avoided, and it has higher safety and environmental protection, and is more suitable for application in the medical field. In addition, the preparation method of the present invention has a simple process, is easy to operate, and is low in cost, and has higher economic and social benefits.
具体实施方式DETAILED DESCRIPTION
下面将结合本发明具体实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例；基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solution of the present invention will be clearly and completely described below in conjunction with specific embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
本发明提供了一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：The present invention provides a non-bisphenol A type medical polycarbonate, comprising the following components in percentage by mass:
非双酚A型二酚化合物：50-70wt％；Non-bisphenol A type diphenol compound: 50-70wt%;
碳酸二酯类化合物：20-40wt％；Carbonic acid diester compounds: 20-40wt%;
封端剂：1-5wt％；Capping agent: 1-5wt%;
催化剂：0.01-0.1wt％。Catalyst: 0.01-0.1wt%.
本实施例的非双酚A型二酚化合物为对苯二酚、间苯二酚、联苯二酚中的一种。The non-bisphenol A type diphenol compound of this embodiment is one of hydroquinone, resorcinol and biphenol.
本实施例的碳酸二酯类化合物为碳酸二苯酯、碳酸二甲酯、碳酸二乙酯中的一种。The carbonic acid diester compound of this embodiment is one of diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
本实施例的封端剂为对枯基苯酚、二枯基苯酚、对叔丁基苯酚中的一种。The end-capping agent of this embodiment is one of p-cumylphenol, dicumylphenol and p-tert-butylphenol.
本实施例的催化剂为四丁基溴化铵、三苯基膦中的一种。The catalyst in this embodiment is one of tetrabutylammonium bromide and triphenylphosphine.
一种非双酚A型医用聚碳酸酯的制备工艺，包括以下步骤：A preparation process of non-bisphenol A type medical polycarbonate comprises the following steps:
S1：将非双酚A型二酚化合物、碳酸二芳基酯、封端剂和催化剂按照上述成分比例混合均匀，得到反应混合物；S1: uniformly mixing a non-bisphenol A type diphenol compound, a diaryl carbonate, a capping agent and a catalyst according to the above-mentioned component ratio to obtain a reaction mixture;
S2：将反应混合物加入熔融酯交换反应器中，在氮气保护下进行熔融酯交换反应；S2: adding the reaction mixture into a melt transesterification reactor, and performing a melt transesterification reaction under nitrogen protection;
S3：将熔融酯交换反应后的产物进行固液分离，得到固相产物和液相产物。S3: performing solid-liquid separation on the product after the melt transesterification reaction to obtain a solid phase product and a liquid phase product.
S4：将固相产物进行真空干燥处理，得到干燥后的聚碳酸酯粗品；S4: vacuum drying the solid phase product to obtain a dried crude polycarbonate product;
S5：将干燥后的聚碳酸酯粗品进行熔融挤出处理，熔融挤出机的长径比为30-50:1，熔融温度为250-300℃，得到熔融挤出后的聚碳酸酯；S5: melt-extrude the dried crude polycarbonate, wherein the aspect ratio of the melt extruder is 30-50:1 and the melting temperature is 250-300° C. to obtain the polycarbonate after melt extrusion;
S6：将熔融挤出后的聚碳酸酯进行冷却切粒处理，得到最终的非双酚A型医用聚碳酸酯产品。S6: Cooling and pelletizing the melt-extruded polycarbonate to obtain a final non-bisphenol A medical polycarbonate product.
本实施例的S2中，熔融酯交换反应，反应温度为200-250℃，反应时间为2-4h。In S2 of this embodiment, the melt transesterification reaction has a reaction temperature of 200-250° C. and a reaction time of 2-4 h.
本实施例的S4中，干燥温度为100-120℃，干燥时间为2-4h。In S4 of this embodiment, the drying temperature is 100-120° C. and the drying time is 2-4 hours.
实施例1：Embodiment 1:
一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：A non-bisphenol A medical polycarbonate comprising the following components in percentage by mass:
非双酚A型二酚化合物：50wt％；Non-bisphenol A type diphenol compound: 50wt%;
碳酸二酯类化合物：20wt％；Carbonic acid diester compounds: 20wt%;
封端剂：1wt％；Capping agent: 1wt%;
催化剂：0.01wt％。Catalyst: 0.01 wt%.
本实施例的非双酚A型二酚化合物为对苯二酚、间苯二酚、联苯二酚中的一种。The non-bisphenol A type diphenol compound of this embodiment is one of hydroquinone, resorcinol and biphenol.
本实施例的碳酸二酯类化合物为碳酸二苯酯、碳酸二甲酯、碳酸二乙酯中的一种。The carbonic acid diester compound of this embodiment is one of diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
本实施例的封端剂为对枯基苯酚、二枯基苯酚、对叔丁基苯酚中的一种。The end-capping agent of this embodiment is one of p-cumylphenol, dicumylphenol and p-tert-butylphenol.
本实施例的催化剂为四丁基溴化铵、三苯基膦中的一种。The catalyst in this embodiment is one of tetrabutylammonium bromide and triphenylphosphine.
一种非双酚A型医用聚碳酸酯的制备工艺，包括以下步骤：A preparation process of non-bisphenol A type medical polycarbonate comprises the following steps:
S1：将非双酚A型二酚化合物、碳酸二芳基酯、封端剂和催化剂按照上述成分比例混合均匀，得到反应混合物；S1: uniformly mixing a non-bisphenol A type diphenol compound, a diaryl carbonate, a capping agent and a catalyst according to the above-mentioned component ratio to obtain a reaction mixture;
S2：将反应混合物加入熔融酯交换反应器中，在氮气保护下进行熔融酯交换反应；S2: adding the reaction mixture into a melt transesterification reactor, and performing a melt transesterification reaction under nitrogen protection;
S3：将熔融酯交换反应后的产物进行固液分离，得到固相产物和液相产物。S3: performing solid-liquid separation on the product after the melt transesterification reaction to obtain a solid phase product and a liquid phase product.
S4：将固相产物进行真空干燥处理，得到干燥后的聚碳酸酯粗品；S4: vacuum drying the solid phase product to obtain a dried crude polycarbonate product;
S5：将干燥后的聚碳酸酯粗品进行熔融挤出处理，熔融挤出机的长径比为30:1，熔融温度为250℃，得到熔融挤出后的聚碳酸酯；S5: subjecting the dried crude polycarbonate to melt extrusion, wherein the aspect ratio of the melt extruder is 30:1 and the melting temperature is 250° C., to obtain a polycarbonate after melt extrusion;
S6：将熔融挤出后的聚碳酸酯进行冷却切粒处理，得到最终的非双酚A型医用聚碳酸酯产品。S6: Cooling and pelletizing the melt-extruded polycarbonate to obtain a final non-bisphenol A medical polycarbonate product.
本实施例的S2中，熔融酯交换反应，反应温度为200℃，反应时间为2h。In S2 of this embodiment, the melt transesterification reaction has a reaction temperature of 200° C. and a reaction time of 2 h.
本实施例的S4中，干燥温度为100℃，干燥时间为2h。In S4 of this embodiment, the drying temperature is 100° C. and the drying time is 2 hours.
实施例2：Embodiment 2:
一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：A non-bisphenol A medical polycarbonate comprising the following components in percentage by mass:
非双酚A型二酚化合物：70wt％；Non-bisphenol A type diphenol compound: 70wt%;
碳酸二酯类化合物：40wt％；Carbonic acid diester compounds: 40wt%;
封端剂：5wt％；Capping agent: 5wt%;
催化剂：0.1wt％。Catalyst: 0.1 wt%.
本实施例的非双酚A型二酚化合物为对苯二酚、间苯二酚、联苯二酚中的一种。The non-bisphenol A type diphenol compound of this embodiment is one of hydroquinone, resorcinol and biphenol.
本实施例的碳酸二酯类化合物为碳酸二苯酯、碳酸二甲酯、碳酸二乙酯中的一种。The carbonic acid diester compound of this embodiment is one of diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
本实施例的封端剂为对枯基苯酚、二枯基苯酚、对叔丁基苯酚中的一种。The end-capping agent of this embodiment is one of p-cumylphenol, dicumylphenol and p-tert-butylphenol.
本实施例的催化剂为四丁基溴化铵、三苯基膦中的一种。The catalyst in this embodiment is one of tetrabutylammonium bromide and triphenylphosphine.
一种非双酚A型医用聚碳酸酯的制备工艺，包括以下步骤：A preparation process of non-bisphenol A type medical polycarbonate comprises the following steps:
S1：将非双酚A型二酚化合物、碳酸二芳基酯、封端剂和催化剂按照上述成分比例混合均匀，得到反应混合物；S1: uniformly mixing a non-bisphenol A type diphenol compound, a diaryl carbonate, a capping agent and a catalyst according to the above-mentioned component ratio to obtain a reaction mixture;
S2：将反应混合物加入熔融酯交换反应器中，在氮气保护下进行熔融酯交换反应；S2: adding the reaction mixture into a melt transesterification reactor, and performing a melt transesterification reaction under nitrogen protection;
S3：将熔融酯交换反应后的产物进行固液分离，得到固相产物和液相产物。S3: performing solid-liquid separation on the product after the melt transesterification reaction to obtain a solid phase product and a liquid phase product.
S4：将固相产物进行真空干燥处理，得到干燥后的聚碳酸酯粗品；S4: vacuum drying the solid phase product to obtain a dried crude polycarbonate product;
S5：将干燥后的聚碳酸酯粗品进行熔融挤出处理，熔融挤出机的长径比为50:1，熔融温度为300℃，得到熔融挤出后的聚碳酸酯；S5: subjecting the dried crude polycarbonate to melt extrusion, wherein the aspect ratio of the melt extruder is 50:1 and the melting temperature is 300° C., to obtain a polycarbonate after melt extrusion;
S6：将熔融挤出后的聚碳酸酯进行冷却切粒处理，得到最终的非双酚A型医用聚碳酸酯产品。S6: Cooling and pelletizing the melt-extruded polycarbonate to obtain a final non-bisphenol A medical polycarbonate product.
本实施例的S2中，熔融酯交换反应，反应温度为250℃，反应时间为4h。In S2 of this embodiment, the melt transesterification reaction is carried out at a reaction temperature of 250° C. and a reaction time of 4 h.
本实施例的S4中，干燥温度为120℃，干燥时间为4h。In S4 of this embodiment, the drying temperature is 120° C. and the drying time is 4 hours.
实施例3：Embodiment 3:
一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：A non-bisphenol A medical polycarbonate comprising the following components in percentage by mass:
非双酚A型二酚化合物：60wt％；Non-bisphenol A type diphenol compound: 60wt%;
碳酸二酯类化合物：30wt％；Carbonic acid diester compounds: 30wt%;
封端剂：3wt％；Capping agent: 3wt%;
催化剂：0.05wt％。Catalyst: 0.05wt%.
本实施例的非双酚A型二酚化合物为对苯二酚、间苯二酚、联苯二酚中的一种。The non-bisphenol A type diphenol compound of this embodiment is one of hydroquinone, resorcinol and biphenol.
本实施例的碳酸二酯类化合物为碳酸二苯酯、碳酸二甲酯、碳酸二乙酯中的一种。The carbonic acid diester compound of this embodiment is one of diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
本实施例的封端剂为对枯基苯酚、二枯基苯酚、对叔丁基苯酚中的一种。The end-capping agent of this embodiment is one of p-cumylphenol, dicumylphenol and p-tert-butylphenol.
本实施例的催化剂为四丁基溴化铵、三苯基膦中的一种。The catalyst in this embodiment is one of tetrabutylammonium bromide and triphenylphosphine.
一种非双酚A型医用聚碳酸酯的制备工艺，包括以下步骤：A preparation process of non-bisphenol A type medical polycarbonate comprises the following steps:
S1：将非双酚A型二酚化合物、碳酸二芳基酯、封端剂和催化剂按照上述成分比例混合均匀，得到反应混合物；S1: uniformly mixing a non-bisphenol A type diphenol compound, a diaryl carbonate, a capping agent and a catalyst according to the above-mentioned component ratio to obtain a reaction mixture;
S2：将反应混合物加入熔融酯交换反应器中，在氮气保护下进行熔融酯交换反应；S2: adding the reaction mixture into a melt transesterification reactor, and performing a melt transesterification reaction under nitrogen protection;
S3：将熔融酯交换反应后的产物进行固液分离，得到固相产物和液相产物。S3: performing solid-liquid separation on the product after the melt transesterification reaction to obtain a solid phase product and a liquid phase product.
S4：将固相产物进行真空干燥处理，得到干燥后的聚碳酸酯粗品；S4: vacuum drying the solid phase product to obtain a dried crude polycarbonate product;
S5：将干燥后的聚碳酸酯粗品进行熔融挤出处理，熔融挤出机的长径比为40:1，熔融温度为275℃，得到熔融挤出后的聚碳酸酯；S5: subjecting the dried crude polycarbonate to melt extrusion, wherein the aspect ratio of the melt extruder is 40:1 and the melting temperature is 275° C., to obtain a polycarbonate after melt extrusion;
S6：将熔融挤出后的聚碳酸酯进行冷却切粒处理，得到最终的非双酚A型医用聚碳酸酯产品。S6: Cooling and pelletizing the melt-extruded polycarbonate to obtain a final non-bisphenol A medical polycarbonate product.
本实施例的S2中，熔融酯交换反应，反应温度为225℃，反应时间为3h。In S2 of this embodiment, the melt transesterification reaction is carried out at a reaction temperature of 225° C. and a reaction time of 3 h.
本实施例的S4中，干燥温度为110℃，干燥时间为3h。In S4 of this embodiment, the drying temperature is 110° C. and the drying time is 3 hours.
实施例4：Embodiment 4:
一种非双酚A型医用聚碳酸酯，包括以下质量百分比的成分：A non-bisphenol A medical polycarbonate comprising the following components in percentage by mass:
非双酚A型二酚化合物：55wt％；Non-bisphenol A type diphenol compound: 55wt%;
碳酸二酯类化合物：25wt％；Carbonic acid diester compounds: 25wt%;
封端剂：2wt％；Capping agent: 2wt%;
催化剂：0.03wt％。Catalyst: 0.03wt%.
本实施例的非双酚A型二酚化合物为对苯二酚、间苯二酚、联苯二酚中的一种。The non-bisphenol A type diphenol compound of this embodiment is one of hydroquinone, resorcinol and biphenol.
本实施例的碳酸二酯类化合物为碳酸二苯酯、碳酸二甲酯、碳酸二乙酯中的一种。The carbonic acid diester compound of this embodiment is one of diphenyl carbonate, dimethyl carbonate and diethyl carbonate.
本实施例的封端剂为对枯基苯酚、二枯基苯酚、对叔丁基苯酚中的一种。The end-capping agent of this embodiment is one of p-cumylphenol, dicumylphenol and p-tert-butylphenol.
本实施例的催化剂为四丁基溴化铵、三苯基膦中的一种。The catalyst in this embodiment is one of tetrabutylammonium bromide and triphenylphosphine.
一种非双酚A型医用聚碳酸酯的制备工艺，包括以下步骤：A preparation process of non-bisphenol A type medical polycarbonate comprises the following steps:
S1：将非双酚A型二酚化合物、碳酸二芳基酯、封端剂和催化剂按照上述成分比例混合均匀，得到反应混合物；S1: uniformly mixing a non-bisphenol A type diphenol compound, a diaryl carbonate, a capping agent and a catalyst according to the above-mentioned component ratio to obtain a reaction mixture;
S2：将反应混合物加入熔融酯交换反应器中，在氮气保护下进行熔融酯交换反应；S2: adding the reaction mixture into a melt transesterification reactor, and performing a melt transesterification reaction under nitrogen protection;
S3：将熔融酯交换反应后的产物进行固液分离，得到固相产物和液相产物。S3: performing solid-liquid separation on the product after the melt transesterification reaction to obtain a solid phase product and a liquid phase product.
S4：将固相产物进行真空干燥处理，得到干燥后的聚碳酸酯粗品；S4: vacuum drying the solid phase product to obtain a dried crude polycarbonate product;
S5：将干燥后的聚碳酸酯粗品进行熔融挤出处理，熔融挤出机的长径比为35:1，熔融温度为260℃，得到熔融挤出后的聚碳酸酯；S5: subjecting the dried crude polycarbonate to melt extrusion, wherein the aspect ratio of the melt extruder is 35:1 and the melting temperature is 260° C., to obtain a polycarbonate after melt extrusion;
S6：将熔融挤出后的聚碳酸酯进行冷却切粒处理，得到最终的非双酚A型医用聚碳酸酯产品。S6: Cooling and pelletizing the melt-extruded polycarbonate to obtain a final non-bisphenol A medical polycarbonate product.
本实施例的S2中，熔融酯交换反应，反应温度为210℃，反应时间为2.5h。In S2 of this embodiment, the melt transesterification reaction was carried out at a reaction temperature of 210° C. and a reaction time of 2.5 h.
本实施例的S4中，干燥温度为105℃，干燥时间为2.5h。In S4 of this embodiment, the drying temperature is 105° C. and the drying time is 2.5 h.
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims (8)
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| CN1926170A (en) * | 2004-02-27 | 2007-03-07 | 通用电气公司 | Liquid crystal polycarbonates and methods of preparing same |
| US20070100118A1 (en) * | 2005-10-28 | 2007-05-03 | Gautam Chatterjee | Methods for preparing transparent articles from hydroquinone polycarbonate copolymers |
| CN111349223A (en) * | 2020-05-07 | 2020-06-30 | 中国科学院过程工程研究所 | A kind of composite catalyst for synthesizing polycarbonate by transesterification method and preparation method of polycarbonate intermediate |
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| JPH07126373A (en) * | 1993-11-04 | 1995-05-16 | Idemitsu Kosan Co Ltd | Polycarbonate manufacturing method |
| CN1926170A (en) * | 2004-02-27 | 2007-03-07 | 通用电气公司 | Liquid crystal polycarbonates and methods of preparing same |
| US20070100118A1 (en) * | 2005-10-28 | 2007-05-03 | Gautam Chatterjee | Methods for preparing transparent articles from hydroquinone polycarbonate copolymers |
| CN111349223A (en) * | 2020-05-07 | 2020-06-30 | 中国科学院过程工程研究所 | A kind of composite catalyst for synthesizing polycarbonate by transesterification method and preparation method of polycarbonate intermediate |
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