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Preparation of 2,4,6-trinitroresorcinol

A technology of trinitroresorcinol and resorcinol, which is applied in 2 fields, can solve the problems of long production cycle, large amount of waste acid waste water, and large amount of acid used, and achieves reduced production costs, simple operation, and high reaction rate. short time effect

Inactive Publication Date: 2009-06-24
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method: 1. The amount of acid used is large, and the amount of waste acid waste water is large, which is not conducive to environmental protection; 2. The production cycle is long, the energy consumption is large, and the product contains many impurities

Method used

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  • Preparation of 2,4,6-trinitroresorcinol
  • Preparation of 2,4,6-trinitroresorcinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 0.1101g (1mmol) of resorcinol and 1mL of 50% acetic acid to a 50mL Erlenmeyer flask. Dissolve 0.548g (1mmol) of cerium ammonium nitrate in 4mL of water to obtain an aqueous solution of cerium ammonium nitrate. Under magnetic stirring, add cerium ammonium nitrate dropwise. The aqueous solution was heated to 30°C and reacted for 0.8h. The reactants were completely converted into products (TLC tracking, ethyl acetate: petroleum ether = 2:1), and the stirring was stopped; the product was poured into ice water, and a brownish-red solid precipitated; Suction filtration, washing the precipitate with distilled water twice to obtain 2,4,6-trinitroresorcinol. Weighing: 0.18g, yield: 73.5%, measured melting point: 178°C-179.5°C, IR: v max (KBr tablet, cm -1 ), 3131, 1671, 1506, 1400, 850.6; UV: (anhydrous methanol) λ max : 252.3; MS: m / z(M-H) + : 245.7; 1 HNMR: (DMSO-d 6 , Ppm) δ: 6.31 (s, 2H), 9.16 (s, 1H).

Embodiment 2

[0013] In a 50mL Erlenmeyer flask, add 0.5505g (5mmol) resorcinol and 5mL 25% acetic acid, 3.562g (6.5mmol) cerium ammonium nitrate dissolved in 20mL of water to obtain cerium ammonium nitrate aqueous solution, under magnetic stirring, add cerium nitrate dropwise Aqueous ammonium solution, heated to 45℃, reacted for 1.2h, the reactant was completely converted into product (TLC tracking, ethyl acetate: petroleum ether = 2:1), stop stirring; pour the product into ice water, a brownish-red solid precipitated ; Suction filtration, distilled water washing precipitation 3 times to obtain 2,4,6-trinitroresorcinol. Weighing: 0.882g, yield: 72%, measured melting point: 178.5℃-179.6℃, IR: v max (KBr tablet, cm -1 ), 3130, 1670, 1504, 1400, 850.6; UV: (anhydrous methanol) λ max : 252.5; MS: m / z(M-H) + : 245.7; 1 HNMR: (DMSO-d 6 , Ppm) δ: 6.30 (s, 2H), 9.19 (s, 1H).

Embodiment 3

[0015] Add 66.061g (600mmol) of resorcinol and 60mL of 5% acetic acid in a 1500mL round bottom flask, and dissolve 526.08g (960mmol) of cerium ammonium nitrate in 550mL of water to obtain an aqueous solution of cerium ammonium nitrate. Under magnetic stirring, add cerium nitrate dropwise. Aqueous ammonium solution, heated to 60℃, reacted for 1.6h, the reactant was completely converted into product (TLC tracking, ethyl acetate: petroleum ether = 2:1), stop stirring; pour the product into ice water, a brownish-red solid precipitated ; Suction filtration, distilled water washing precipitation 3 times to obtain 2,4,6-trinitroresorcinol. Weighing: 120.69g, yield: 82.1%, measured melting point: 178.1℃-179.4℃, IR: v max (KBr tablet, cm -1 ), 3132, 1671, 1505, 1401, 851.2; UV: (anhydrous methanol) λ max : 253.1; MS: m / z(M-H) + : 245.6; 1 HNMR: (DMSO-d 6 , Ppm) δ: 6.29 (s, 2H), 9.18 (s, 1H).

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Abstract

The invention discloses a method for preparing 2, 4, 6-trinitroresorein; firstly, resorcinol is dissolved in acetic acid with volume concentration of 5%-50%; by magnetic stirring, ammonium ceric nitrate water solution is added in and the obtained solution is heated to the temperature of 30-60 DEG C; the mol ratio of the reactants of resorcinol, ammonium ceric nitrate and water is 1:1.6:0.05-0.22, and the reaction lasts for 0.8-1.6h; when the reactants are fully converted into products (TLC tracking, ethyl acetate: ligarine=2:1), the stirring is stopped; the products are poured into ice water and brownish red solid matters are separated out; after suction filtration, distillation, water rinse and precipitation of 2-3 times, 2, 4, 6-trinitroresorein is obtained. The method of the invention adopts environmental-friendly chemical ammonium ceric nitrate as nitrating reagent, the operation is convenient, the reaction period is short and the production cost is reduced.

Description

Technical field [0001] The invention relates to a preparation method of a compound, in particular to a preparation method of 2,4,6-trinitroresorcinol. Background technique [0002] 2,4,6-Trinitroresorcinol, also known as stilbene acid or astringent acid, is a raw material for the manufacture of heavy metal salts of trinitroresorcinol, and can also be used as a component and analytical reagent for explosives Wait. The preparation method of 2,4,6-trinitroresorcinol includes the nitration phenol method. The resorcinol is first sulfonated, then nitrated, and finally hydrolyzed to obtain the product. But this method: 1. The amount of acid used is large, and the amount of waste acid wastewater is large, which is not conducive to environmental protection; 2. The production cycle is long, the energy consumption is large, and the product contains many impurities. Summary of the invention [0003] The purpose of the present invention is to provide a preparation method of 2,4,6-trinitrores...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/24C07C201/08
Inventor 朱惠琴周建峰支三军
Owner HUAIYIN TEACHERS COLLEGE
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