AB type modified poly-p-phenylene terephthamide (PPTA) monomer and preparation and applications thereof
A technology of reaction and reaction vessel, which is applied in the field of preparing modified PPTA resin and fiber, and can solve problems such as poor thermal performance and limited application range
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Embodiment 1
[0095] Example 1 Preparation of methyl 2-hydroxy-4-carboxybenzoate (α-MHT)
[0096] (1) Preparation of dimethyl hydroxyterephthalate (DMHT)
[0097] Add 15.00g hydroxyterephthalic acid (HTA) (0.082mol), 150mL methanol, 24.1mL SOCl to the reaction vessel 2 (0.330mol), heated, stirred, refluxed and reacted for 21h, poured into a large amount of ice water after cooling, separated out a white precipitate, adjusted to pH=8 with dilute ammonia water and filtered, and the filter cake was recrystallized with methanol to obtain 16.21g of white needle-like DMHT with a purity of 99.1%. Yield 94.16%.
[0098] (2) Preparation of α-MHT
[0099] Add 6.30 g (0.030 mol) DMHT and 200 mL of 5.00 g NaOH (0.120 mol) aqueous solution to the reaction vessel, stir in an ice-water bath, react at 0~5 °C for 60 min, pour it into a beaker, adjust the pH to 8 with dilute hydrochloric acid, filter out the insoluble The filtrate was added with dilute hydrochloric acid to pH=4.4, filtered, and the filter ...
Embodiment 2~7
[0100] The preparation of embodiment 2~7 DMHT and α-MHT
[0101] (1) Preparation of dimethyl hydroxyterephthalate (DMHT)
[0102] DMHT was synthesized by the same operation as Example 1-(1), according to the parameter range described in Table 1 (different dosages of SOCl 2 and different reaction times) to carry out experiments with different parameters, the results are shown in Table 1:
[0103] Table 1:
[0104] Example SOCl 2 equivalent Reflux time / h product purity / % Yield / % 2 2.99 7.5 DMHT 96.3 83.5 3 3.50 15 DMHT 98.6 89.4 Comparative Example 1 1.5 0.5 β-Monoester 94.7 69.3
[0105] (2) Preparation of α-MHT
[0106] Adopt the same operation as Example 1-(2) to synthesize α-MHT, and carry out experiments with different parameters according to the parameter range (temperature, alkali dosage reaction time, hydrolysis solvent) described in Table 2, and the results are shown in Table 2:
[0107] Table 2:
[0108]...
Embodiment 8
[0109] Example 8 AB-type new monomers 4-(4-amino-3-methylanilinecarbonyl)-2-hydroxybenzoic acid (AMHBA) and 4-(4-amino-3-methylanilinecarbonyl)-2-hydroxyl Synthesis of methyl benzoate (MAMHB)
[0110] (1) Preparation of 4-(4-amino-3-methylanilinecarbonyl)-2-hydroxy-benzoic acid methyl ester (MAMHB):
[0111] Take 0.72 g (0.0033 mol) α-MHT (purity 98.8%) in the reaction vessel, add 25 mL of thionyl chloride, heat to reflux (about 78°C) and dissolve into 3-hydroxy-4-methoxycarbonylbenzyl Acid chloride (3,4-HMBC) in THF, poured into a 50 mL constant pressure burette. Add 0.50 g (0.0041 mol) of 2-methyl-p-phenylenediamine (MPPD) and 10 mL of tetrahydrofuran to a four-necked flask, add 3,4-HMBC THF solution dropwise in an ice bath, and react at room temperature (T=26°C) for 12 h, cooled and filtered, the filter cake was treated with ammonia water and dried to obtain 0.82 g of light yellow MAMHB (purity 94.67%, yield 79.38%). The infrared spectrum of MAMHB can be found in figur...
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