CN108947987A - 一种高品质的电子级异氰尿酸三缩水甘油酯 - Google Patents
一种高品质的电子级异氰尿酸三缩水甘油酯 Download PDFInfo
- Publication number
- CN108947987A CN108947987A CN201810592437.7A CN201810592437A CN108947987A CN 108947987 A CN108947987 A CN 108947987A CN 201810592437 A CN201810592437 A CN 201810592437A CN 108947987 A CN108947987 A CN 108947987A
- Authority
- CN
- China
- Prior art keywords
- alkali
- glycidyl ester
- epoxychloropropane
- isocyanuric acid
- vacuum
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000003513 alkali Substances 0.000 claims abstract description 46
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002425 crystallisation Methods 0.000 claims abstract description 19
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000007790 solid phase Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000012452 mother liquor Substances 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 230000006837 decompression Effects 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000004593 Epoxy Substances 0.000 claims description 4
- -1 chloropropionate Alkane Chemical class 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000010025 steaming Methods 0.000 claims description 4
- 238000007259 addition reaction Methods 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- OUPZKGBUJRBPGC-UHFFFAOYSA-N 1,3,5-tris(oxiran-2-ylmethyl)-1,3,5-triazinane-2,4,6-trione Chemical compound O=C1N(CC2OC2)C(=O)N(CC2OC2)C(=O)N1CC1CO1 OUPZKGBUJRBPGC-UHFFFAOYSA-N 0.000 abstract description 45
- 239000000047 product Substances 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000007363 ring formation reaction Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 5
- 230000007423 decrease Effects 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract description 3
- 229910052736 halogen Inorganic materials 0.000 abstract description 3
- 150000002367 halogens Chemical class 0.000 abstract description 3
- 238000004321 preservation Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 9
- 239000007788 liquid Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002924 oxiranes Chemical class 0.000 description 4
- 238000012797 qualification Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000007142 ring opening reaction Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005292 vacuum distillation Methods 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- YWNYZQTZOONLGU-UHFFFAOYSA-N C(CC)Cl.[O] Chemical compound C(CC)Cl.[O] YWNYZQTZOONLGU-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- VIRPUNZTLGQDDV-UHFFFAOYSA-N chloro propanoate Chemical compound CCC(=O)OCl VIRPUNZTLGQDDV-UHFFFAOYSA-N 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- HPOKESDSMZRZLC-UHFFFAOYSA-N propan-2-one;hydrochloride Chemical compound Cl.CC(C)=O HPOKESDSMZRZLC-UHFFFAOYSA-N 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D405/00—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom
- C07D405/14—Heterocyclic compounds containing both one or more hetero rings having oxygen atoms as the only ring hetero atoms, and one or more rings having nitrogen as the only ring hetero atom containing three or more hetero rings
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Plural Heterocyclic Compounds (AREA)
Abstract
Description
组别 | 平均环氧值 | 合格率 |
组1 | 1.02 | 100% |
组2 | 1.04 | 100% |
组3 | 1.03 | 100% |
组4 | 1.05 | 100% |
组5 | 1.03 | 100% |
组6 | 1.03 | 100% |
组7 | 1.05 | 100% |
组8 | 1.04 | 100% |
组9 | 1.03 | 100% |
组10 | 1.03 | 100% |
组11 | 1.03 | 100% |
组12 | 1.06 | 66.7% |
组13 | 1.03 | 100% |
组14 | 1.04 | 100% |
组15 | 1.05 | 100% |
组16 | 1.04 | 100% |
组17 | 1.06 | 66.7% |
组18 | 1.04 | 100% |
组19 | 1.03 | 100% |
组20 | 1.04 | 100% |
组21 | 1.03 | 100% |
组22 | 1.03 | 100% |
组23 | 1.05 | 100% |
对比例1 | 1.06 | 66.7% |
对比例2 | 1.04 | 100% |
组别 | 生产TGIC(t) | 产率(%) |
组1 | 2.07 | 94.09 |
组2 | 2.05 | 93.12 |
组3 | 2.06 | 93.75 |
组4 | 1.98 | 90.01 |
组5 | 2.07 | 94.01 |
组6 | 2.07 | 94.00 |
组7 | 1.96 | 89.24 |
组8 | 2.06 | 93.56 |
组9 | 2.05 | 93.01 |
组10 | 2.07 | 94.00 |
组11 | 2.07 | 94.01 |
组12 | 1.84 | 83.69 |
组13 | 2.06 | 93.55 |
组14 | 2.06 | 93.68 |
组15 | 2.03 | 92.11 |
组16 | 2.07 | 94.05 |
组17 | 1.81 | 82.17 |
组18 | 2.07 | 94.02 |
组19 | 2.07 | 94.05 |
组20 | 2.07 | 94.01 |
组21 | 2.07 | 94.02 |
组22 | 2.07 | 94.02 |
组23 | 2.07 | 93.89 |
对比例1 | 1.94 | 88.12 |
对比例2 | 1.99 | 90.33 |
Claims (7)
Priority Applications (1)
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CN201810592437.7A CN108947987B (zh) | 2018-06-11 | 2018-06-11 | 一种高品质的电子级异氰尿酸三缩水甘油酯 |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112321576A (zh) * | 2020-11-25 | 2021-02-05 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的制备方法 |
CN113105438A (zh) * | 2021-04-09 | 2021-07-13 | 河南易交联新材料科技有限公司 | 一种高纯度三(环氧丙基)异氰尿酸酯的合成方法 |
CN113278014A (zh) * | 2021-06-04 | 2021-08-20 | 黄山华惠科技有限公司 | 一种低氯电子级tgic及其制备方法 |
CN114315810A (zh) * | 2020-09-29 | 2022-04-12 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的纯化方法 |
CN114315809A (zh) * | 2020-09-29 | 2022-04-12 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的制备方法 |
CN114957225A (zh) * | 2021-07-31 | 2022-08-30 | 安徽诗雅涤科技有限公司 | 一种led电子封装专用环氧树脂的制备方法及其环氧树脂 |
CN118496214A (zh) * | 2024-07-17 | 2024-08-16 | 黄山华惠科技有限公司 | 一种异氰脲酸三缩水甘油酯的制备方法 |
Citations (3)
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JPS5328916B2 (zh) * | 1974-06-17 | 1978-08-17 | ||
CN101333285A (zh) * | 2008-07-24 | 2008-12-31 | 中昊晨光化工研究院 | 制备苯酚甲醛型环氧树脂的方法 |
US20150232458A1 (en) * | 2014-02-20 | 2015-08-20 | Piramal Enterprises Limited | Process for preparation of triglycidyl isocyanurate (tgic) |
-
2018
- 2018-06-11 CN CN201810592437.7A patent/CN108947987B/zh active Active
Patent Citations (3)
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JPS5328916B2 (zh) * | 1974-06-17 | 1978-08-17 | ||
CN101333285A (zh) * | 2008-07-24 | 2008-12-31 | 中昊晨光化工研究院 | 制备苯酚甲醛型环氧树脂的方法 |
US20150232458A1 (en) * | 2014-02-20 | 2015-08-20 | Piramal Enterprises Limited | Process for preparation of triglycidyl isocyanurate (tgic) |
Non-Patent Citations (1)
Title |
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艾武全,等: "季铵碱催化体系下异氰尿酸三缩水甘油酯的合成及性能", 《电镀与涂饰》 * |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114315810A (zh) * | 2020-09-29 | 2022-04-12 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的纯化方法 |
CN114315809A (zh) * | 2020-09-29 | 2022-04-12 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的制备方法 |
CN114315810B (zh) * | 2020-09-29 | 2023-12-15 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的纯化方法 |
CN114315809B (zh) * | 2020-09-29 | 2023-12-15 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的制备方法 |
CN112321576A (zh) * | 2020-11-25 | 2021-02-05 | 湖南云科化工有限公司 | 一种异氰尿酸三缩水甘油酯的制备方法 |
CN113105438A (zh) * | 2021-04-09 | 2021-07-13 | 河南易交联新材料科技有限公司 | 一种高纯度三(环氧丙基)异氰尿酸酯的合成方法 |
CN113278014A (zh) * | 2021-06-04 | 2021-08-20 | 黄山华惠科技有限公司 | 一种低氯电子级tgic及其制备方法 |
CN113278014B (zh) * | 2021-06-04 | 2024-07-05 | 黄山华惠科技有限公司 | 一种低氯电子级tgic及其制备方法 |
CN114957225A (zh) * | 2021-07-31 | 2022-08-30 | 安徽诗雅涤科技有限公司 | 一种led电子封装专用环氧树脂的制备方法及其环氧树脂 |
CN114957225B (zh) * | 2021-07-31 | 2024-05-10 | 安徽诗雅涤科技有限公司 | 一种led电子封装专用环氧树脂的制备方法及其环氧树脂 |
CN118496214A (zh) * | 2024-07-17 | 2024-08-16 | 黄山华惠科技有限公司 | 一种异氰脲酸三缩水甘油酯的制备方法 |
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