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Preparation method for 4,6-diamino resorcinol and 4,6-diamino resorcinol hydrochloride

A technology of diaminoresorcinol hydrochloride and diaminoresorcinol, which is applied in 4 fields, can solve the problems of high requirements for equipment and operators and high cost, and achieve low requirements for equipment and personnel, low cost, and responsiveness The effect of mild conditions

Inactive Publication Date: 2012-03-21
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned processes using resorcinol as raw materials all adopt sulfonation and nitration processes, and all use fuming sulfuric acid, which requires high requirements for equipment and operators
Moreover, catalytic hydrogenation reduction is used in the nitro reduction reaction. In this process, precious metal catalysts such as palladium are used, and high-pressure hydrogenation equipment is used, and the cost is relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 33g (0.3mol) of resorcinol and 100ml of 98% concentrated sulfuric acid were added to a 1000ml four-neck round bottom flask equipped with mechanical stirring, a condenser, a thermometer and an addition funnel. Place the reactor in a water bath and heat it to 45°C, start to add dropwise a mixed acid consisting of 50ml of 68% concentrated nitric acid and 60ml of 98% concentrated sulfuric acid, control the rate of addition for 0.5-1h to complete the dropwise addition, and keep the reaction temperature below 65°C. After the dropwise addition, react at 65°C for 2 hours. After the reaction is completed, add 100ml of deionized water while stirring, keep the temperature at 50°C for 1h, and crystals will gradually precipitate out during the reaction. Cool the mixture to room temperature, and filter out the product. Wash with water until the reactant is neutral to obtain 52.4 g of yellow crude product, dissolve the above 50 g of yellow solid in 200 ml of absolute ethanol, heat to d...

Embodiment 2

[0026] Add 330g resorcinol and 1000ml 98% concentrated sulfuric acid to a 5000ml four-neck round bottom flask equipped with mechanical stirring, condenser, thermometer and addition funnel. Place the reactor in a water bath and heat it to 50°C, start to add dropwise a mixed acid consisting of 550ml of 68% concentrated nitric acid and 600ml of 98% concentrated sulfuric acid, and control the rate of addition for 1 hour to complete the dropwise addition, keeping the reaction temperature below 65°C. After the dropwise addition, react at 65°C for 3 hours. After the reaction is completed, add 1000ml of deionized water while stirring, keep the temperature at 50°C for 1 hour for hydrolysis, the reaction gradually precipitates crystals, cool the mixture to room temperature, and filter out The product was washed with water until the reactant was neutral to obtain 545 g of yellow 4,6-dinitroresorcinol. The above 500g of yellow solid was dissolved in 2000ml of anhydrous methanol, heated to...

Embodiment 3

[0029] 22g (0.2mol) of resorcinol and 80ml of 98% concentrated sulfuric acid were added to a 1000ml four-neck round bottom flask equipped with a mechanical stirrer, a condenser, a thermometer and an addition funnel. Place the reactor in a water bath and heat it to 50°C, start adding dropwise a mixed acid consisting of 40ml of 68% concentrated nitric acid and 50ml of 98% concentrated sulfuric acid, and control the rate of addition for 30 minutes to complete the dropwise addition, keeping the reaction temperature below 75°C. After the dropwise addition, react at 75°C for 3 hours. After the reaction is completed, add 80ml of deionized water while stirring, keep the temperature at 75°C for 2 hours for hydrolysis, the reaction gradually precipitates crystals, cool the mixture to room temperature, and filter out The product was washed with water until the reactant was neutral to obtain 32.4 g of a yellow crude product. The above 30 g yellow solid was dissolved in 150 ml of anhydrous ...

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Abstract

The invention relates to a preparation method for 4,6-diamino resorcinol and 4,6-diamino resorcinol hydrochloride, which belongs to the technical field of high polymer bullet resistant material monomer synthesis and includes the steps of firstly, adding concentrated sulfuric acid serving as base to a nitration reactor, nitrifying resorcinol in mixed acid containing sulfur acid and nitric acid to obtain nitration mixture and then obtaining 4,6-diamino resorcinol by means of recrystallization, and secondly, enabling the 4,6-diamino resorcinol to be reduced prior to being added with concentrated hydrochloric acid, obtaining white crystal, namely, crude 4,6-diamino resorcinol hydrochloride, and then obtaining pure 4,6-diamino resorcinol hydrochloride after recrystallization of hydrochloric acid. The preparation method has mild reaction conditions, and the 4,6-diamino resorcinol serving as intermediate is freely soluble in alcohol solvent such as methanol, ethanol and the like, so that reduction of nitryl is easier. Besides, requirements on equipment and staff are low, and cost is low.

Description

technical field [0001] The invention relates to a preparation method of 4,6-diaminoresorcinol and its hydrochloride, and belongs to the technical field of polymer ballistic material monomer synthesis. Background technique [0002] 4,6-diaminoresorcinol hydrochloride is an important chemical intermediate and a monomer for the synthesis of polymer materials polybenzobisoxazole (PBO). PBO is a super-performance fiber in the 21st century. It has excellent physical and mechanical properties and chemical properties. Its strength and modulus are twice that of Kevlar fibers, and it also has the heat-resistant and flame-resistant properties of meta-aramid fibers, and its physical and chemical properties completely exceed those of Kevlar fibers. Kevlar fiber, which has been a leader in the field of high-performance fibers so far. A PBO filament with a diameter of 1 mm can lift a weight of 450 kg, and its strength is more than 10 times that of steel wire fibers. [0003] There are tw...

Claims

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Application Information

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IPC IPC(8): C07C215/80C07C213/02
Inventor 王虎刘吉平
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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