Page 152 - 《精细化工》2023年第4期

す 40 ࢤす 4 ᱌ ㇫ ㏳ ࡃ ጒ Vol.40, No.4
20 23 Ꭱ 4 ᰵ FINE CHEMICALS Apr. 2023

ߌ㘪ᱽ᫆
倅㔽☚㖇㟠䛇䚛ధࡃ䗨㠜ι⩟㙵ᴾ㘯

1
1
㘎ᰵ 1,2 喑侙Ⴕ侼 喑䍴䩎倅 喑㓮ᔄ♂ 1*
喍1. ๔䔋⤳ጒ๔႓ ㇫㏳ࡃጒపუ䛺◦჋侹ბ ࡃጒ႓䮏喑䓪Ⴎ ๔䔋 116024喠2. ᆞ㺬᫝ࡻ䭟ࡃ㷲ิⵁ⾣
䮏ᰶ䭽ڙथ喑ᆞ㺬 ๗࣌ 030000喎

ᦅ㺮喟В 4-(4-㓌ധ㠜ധ)-2,3-ι⅛ᱯ㥅-1-䚛Ƞ4,4'-ι⅌ι㠜⩟䚛হ 4-⅕ധ㠜䚇ͧ࣌᫆喑䕇䓴͑ₒ̭䨲∂व᜽γ̭
⻺᫝ಸ⮱⅕ധᄮ〜ᱯ㥅㖁㠜㖇㟠䛇䚛喍A-PPEK喎喑䛴⩕ጛ⹧ម᣼䛼☚∂喍DSC喎ᣏ⾣γڣᄦ䬡㠜ι䚇ധ䗨㠜ι
⩟㙵喍DPPH喎⮱ధࡃᕔ㘪ȡⰥ℁λ፥⩕⮱㟠仆ι㘧ధࡃݯ 4,4'-ι⅕ധι㠜ⵉ喍DDS喎喑A-PPEK ⮱ 5%☚๞䛺⍖
Ꮣ喍T d5% 喎᣽倅γ 69.3 Ďȡओใ喑̻ DDS ౕ 400 Ďᬣᔘ䕌ࡴࡻ̺ह喑A-PPEK ౕⰥह⍖Ꮣ̸⮱䉕䛼Ԋ⪆⢴Ϻ
>95%喑䄡ᬻ A-PPEK जВᰶ᩵㼐۠ᄼܳၽధࡃݯ倅⍖̸ܳ㼐喑ღᭀౕ䗨㠜ι⩟㙵ᴾ㘯͚ᒏ᜽㑧䮤⮱䬛䷅ȡ̭㈨
݄჋侹㶕ᬻ喑В A-PPEK ధࡃ DPPH喑Ҁ㈨ڤᰶхᐯ⮱㔽☚ᕔহߍጒ≮ߕᕔ喑ᒀ A-PPEK क़䛼ͧ DPPH 䉕䛼⮱
10%ᬣ喑ధࡃᴾ㘯⮱ T d5% ज䓫 553.2 Ď喑⣨⦰ࡃ䒙अ⍖Ꮣ倅λ჋侹≸䄂㠰డ 380 Ď喑ᰭѻ叼Ꮣज䓫 0.167 Pa·sȡ
ڠ䩛䃺喟䗨㠜ι⩟㙵ᴾ㘯喠ᱯ㥅㖁㠜㖇㟠䛇䚛喠⅕ധᄮ〜喠㔽倅⍖喠ߌ㘪ᱽ᫆
͚ఫܳㆨत喟TQ323喠TQ630 ᪴⡛ᴴ䃳⴮喟A ᪴」㑃त喟1003-5214 (2023) 04-0838-07

Curing of phthalonitrile resin with high-temperature resistant
poly(phthalazinone ether ketone)

1
1,2
1
HU Yue , MA Shoujun , JIAN Xigao , WENG Zhihuan 1
喍1. State Key Laboratory of Fine Chemicals, School of Chemical Engineering, Dalian University of Technology, Dalian
116024, Liaoning, China; 2. Shanxi Xinhua Chemical Defense Equipment Research Institute Co., Ltd., Taiyuan 030000,
Shanxi, China喎

Abstract: A novel amino terminated poly(phthalazinone ether ketone) (A-PPEK) was synthesized from
4-(4-hydroxylphenyl)(2H)-phthalazin-1-one, 4,4'-difluoro benzophenone and 4-aminophenol by a two-step
one pot method, and its curing performance for resorcinol phthalonitrile (DPPH) was then investigated by
differential scanning calorimetry (DSC). Compared with commonly used aromatic diamine curing agent
4,4'-diaminodiphenyl sulfone (DDS), 5% mass loss temperature (T d5% ) of A-PPEK was increased by 69.3 Ď.
Moreover, A-PPEK could still retain more than 95% of its mass at 400 Ď while DDS displayed rapid
sublimation, suggesting that A-PPEK could effectively solve the problem of defects in phthalonitrile resin
caused by the decomposition of small molecule curing agent at high temperature. Data from a series of tests
showed that the system of DPPH cured with A-PPEK exhibited excellent heat resistance and processability.
When A-PPEK content was 10% of DPPH mass, the T d5% of the cured resin reaching 553.2 Ď, the glass transition
temperature higher than the experimental test scope of 380 Ď, and the minimum viscosity up to 0.167 Pa·s.
Key words: phthalonitrile resin; poly(phthalazinone ether ketone); amine termination; high-temperature
resistant; functional materials

䗨㠜ι⩟㙵ᴾ㘯喍PN喎᭜̭ㆨ䛺㺮⮱倅ᕔ㘪☚ ⮱☚⽠Ⴧᕔহ☚⅔ࡃ⽠ჇᕔȠ㔽ࡃ႓ᕔȠ䭨⛰㜗⚱
ధᕔᴾ㘯喑⩞λڣౕధࡃ䓴⼸͚чϔ⩌ᐯय़ਇ੶Ƞ হѻ॥Ⅱ⢴ぶхᐯᕔ㘪 [4-6] ȡ㔹 PN Ό᭜ੜ̭こव㒻
̶ଗ⣜হ䚋㣮⣜ぶϑ㖁㐀Ჱ [1-3] 喑ϻ㔹Ҭᴾ㘯ڤᰶ倅 ప⊤ۈ䭨⛰ᴴ۳喍MIL-STD-2031喎⮱᱗ᩦᕔᰶᱧᴾ

ᩣ⽬ᬒ᱌喟2022-07-19; Ⴧ⩕ᬒ᱌喟2022-10-06; DOI: 10.13550/j.jxhg.20220679
ധ䛾䶦Ⱋ喟పუ㜗♣⻾႓ധ䛾喍51673033喑51873027喎喠͚๛倅ᵎധ᱙⻾ⵁ͇ߎ䉦喍DUT20TD114喎
҉㔲キϸ喟㘎ᰵ喍1993ÿ喎喑ຠ喑ⶂธ⩌喑E-mail喟645912857@qq.comȡ㖁㈨ϧ喟㓮ᔄ♂喍1980ÿ喎喑⩤喑᪆ᢵ喑E-mail喟
zweng@dlut.edu.cnȡ