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Method for processing bromine/phosphorus-containing epoxy resin by using supercritical methyl alcohol

A technology of phosphorus epoxy resin and supercritical methanol, which is applied in chemical instruments and methods, preparation of organic compounds, production of bulk chemicals, etc., can solve the problems of increased difficulty and inability to solve debromination, dephosphorization and detoxification, and secondary pollution and other issues to achieve the effect of resource reuse

Inactive Publication Date: 2014-05-14
FUJIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since bromine / phosphorus-containing epoxy resins are prone to form persistent organic pollutants such as dioxins during incineration, the difficulty of harmless resource disposal of such wastes is greatly increased
Existing bromine / phosphorus-containing epoxy resin treatment methods such as pyrolysis and physical methods cannot solve the problems of debromination, dephosphorization and detoxification, which easily lead to secondary pollution

Method used

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  • Method for processing bromine/phosphorus-containing epoxy resin by using supercritical methyl alcohol
  • Method for processing bromine/phosphorus-containing epoxy resin by using supercritical methyl alcohol
  • Method for processing bromine/phosphorus-containing epoxy resin by using supercritical methyl alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0016] Such as figure 1 As shown, the waste bromine / phosphorous epoxy resin was sheared into fragments with a length of 3-5 cm. Mix the sheared waste bromine / phosphorous epoxy resin and methanol at a solid-to-liquid ratio of 1:5g / mL and add it to the supercritical fluid reactor. After nitrogen gas is introduced for 1-5 minutes, immediately seal the reactor and heat , start timing after the temperature rises to 240 degrees, at this moment, the pressure in the container is controlled at 8MPa by a manual pressurization device, and the heating is stopped after 15 minutes of reaction. After the temperature drops to room temperature, open the reaction kettle, transfer the reactant to a centrifuge tube for centrifugation, wash the solid phase product with methanol, dry and weigh, use a rotary evaporator to recover the methanol in the liquid phase product, and the remaining oil phase product Weighing, the calculation of gas production is obtained by deducting the mass of solid and li...

Embodiment 2

[0019] Such as figure 1 As shown, the waste bromine / phosphorous epoxy resin was sheared into fragments with a length of 3-5 cm. Mix the cut waste bromine / phosphorous epoxy resin and methanol at a solid-to-liquid ratio of 1:20g / mL and add it to the supercritical fluid reactor. After nitrogen gas is introduced for 1-5 minutes, immediately seal the reactor and heat , start timing after the temperature rises to 350 degrees, at this moment, the pressure in the container is controlled at 18MPa by a manual pressurization device, and the heating is stopped after 60 minutes of reaction. After the temperature drops to room temperature, open the reaction kettle, transfer the reactant to a centrifuge tube for centrifugation, wash the solid phase product with methanol, dry and weigh, use a rotary evaporator to recover the methanol in the liquid phase product, and the remaining oil phase product Weighing, the calculation of gas production is obtained by deducting the mass of solid and liqu...

Embodiment 3

[0022] Such as figure 1 As shown, the waste bromine / phosphorous epoxy resin was sheared into fragments with a length of 3-5 cm. Mix the sheared waste bromine / phosphorous epoxy resin and methanol at a solid-to-liquid ratio of 1:40g / mL and add it to the supercritical fluid reactor. After nitrogen gas is introduced for 1-5 minutes, immediately seal the reactor and heat , start timing after the temperature rises to 400 degrees, at this moment, the pressure in the container is controlled at 22MPa by a manual pressurization device, and the heating is stopped after 120 minutes of reaction. After the temperature drops to room temperature, open the reaction kettle, transfer the reactant to a centrifuge tube for centrifugation, wash the solid phase product with methanol, dry and weigh, use a rotary evaporator to recover the methanol in the liquid phase product, and the remaining oil phase product Weighing, the calculation of gas production is obtained by deducting the mass of solid and...

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Abstract

The invention discloses a method for processing bromine / phosphorus-containing epoxy resin by using supercritical methyl alcohol. The method comprises the following steps: (1) mixing the bromine / phosphorus-containing epoxy resin with the methyl alcohol according to a solid-liquid ratio of 1:5g / mL-1:40g / mL, putting the bromine / phosphorus-containing epoxy resin and the methyl alcohol in a supercritical fluid reaction kettle, adding nitrogen for 1-5 minutes and sealing the supercritical fluid reaction kettle instantly; (2) heating the supercritical fluid reaction kettle, heating to 240-400 DEG C and then starting to time, controlling pressure in a supercritical fluid reaction kettle container to be 8-30MPa through a manual pressing device, reacting for 15-120 minutes and then stopping heating; and (3) cooling to room temperature and then opening the reaction kettle, transferring a reactant to a centrifugal tube to centrifugally separate, washing a solid-phase product by using the methyl alcohol to dry and weigh, recycling the methyl alcohol in a liquid-phase product by using a rotary evaporator, weighing a residual oil-phase product and deducting the mass of solid-liquid products from a total weight of samples to obtain calculation of gas production rate, wherein the recycled methyl alcohol is directly reused as a reaction medium.

Description

technical field [0001] The invention relates to the technical field of recycling and application of printed circuit boards. Specifically, the invention relates to a method for treating bromine / phosphorus-containing epoxy resin in waste printed circuit boards with supercritical methanol. Background technique [0002] Printed circuit boards (PCBs) are the foundation of the electronics industry and are widely used in computers, communication equipment, instrumentation, household appliances and other fields. The average annual growth rate of China's printed circuit board industry is 14.4%. The acceleration of the replacement of electronic and electrical products has led to an increase in the number of discarded PCBs year by year, and the number is very large. Scrap PCBs contain about 70% non-metal and 30% metal. The non-metal part is mainly bromine / phosphorous epoxy resin. The highest content of metal components is copper, in addition to gold, aluminum, nickel, lead, silicon ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/04C07C37/00C07C37/055
CPCC07C37/00C07C37/0555C07C37/52C07C39/04Y02P20/54
Inventor 修福荣齐莹莹
Owner FUJIAN UNIV OF TECH