A kind of solid acetal and preparation method thereof

An acetal, solid technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of large consumption of extractant, cumbersome process, high cost, wide range of uses, few recovery steps and low cost Effect

Active Publication Date: 2022-04-22
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to consume a large amount of extractant and produce more waste liquid, the process is more cumbersome and the cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Waste printed circuit boards are crushed and sorted to collect non-metallic powder. Add 50g of non-metallic powder to 150mL of 5mol / L nitric acid solution, heat at 90°C for 23 hours, filter, adjust the pH of the filtrate to about 3 with sodium hydroxide; stir the filtrate in an environment of 10-15°C and add dropwise After adding 10g of butyraldehyde, continue to stir for 2 hours, then gradually raise the temperature to 50°C, continue to stir and add 0.15g of isopropanol, keep it warm for 2 hours, then raise the temperature to 70°C, and continue to stir for 4 hours.

[0031] After the reaction, cool to room temperature, filter, wash the solid with deionized water, add to 15 mL of 0.5 mol / L sodium hydroxide solution and soak for 2 hours, filter, wash with deionized water three times, and dry to obtain solid acetal.

Embodiment 2

[0033] Waste printed circuit boards are crushed and sorted to collect non-metallic powder. Take 120g of non-metallic powder and add it to 600mL of 7mol / L nitric acid solution, heat at 80°C for 36 hours, filter, adjust the pH of the filtrate to about 1 with sodium carbonate; stir the filtrate in an environment of 10-15°C and add 12g of it dropwise After the addition of benzaldehyde, continue to stir for 2 hours, then gradually heat up to 50°C, continue to stir and add 2.2g of butanol, keep warm for 2 hours, then heat up to 70°C, and continue to stir for 6 hours.

[0034] After the reaction, cool to room temperature, filter, wash the solid with deionized water, add to 20 mL of 1.5 mol / L sodium bicarbonate solution and soak for 3 hours, filter, wash with deionized water three times, and dry to obtain solid acetal.

Embodiment 3

[0036] Waste printed circuit boards are crushed and sorted to collect non-metallic powder. Take 150g of non-metallic powder and add it to 900mL of 6mol / L nitric acid and phosphoric acid (molar ratio is 3:1) solution, heat at 85°C for 30 hours, filter, adjust the pH of the filtrate to about 5 with potassium hydroxide; place the filtrate in 10 Stir in an environment of ~15°C and add 12.9g of valeraldehyde dropwise. After the addition, continue to stir for 1 hour, then gradually raise the temperature to 45°C, continue to stir and add 1.3g of amyl alcohol, keep the temperature for 3 hours, then raise the temperature to 80°C, continue Stir for 5 hours.

[0037] After the reaction, cool to room temperature, filter, wash the solid with deionized water, add to 15 mL of 1.0 mol / L potassium carbonate solution and soak for 3 hours, filter, wash with deionized water three times, and dry to obtain solid acetal.

[0038] In summary, in the present invention, the non-metallic powder obtaine...

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PUM

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Abstract

The invention discloses a solid acetal and a preparation method thereof. The preparation method includes: step 1, crushing and sorting thermosetting epoxy resin waste to obtain non-metal powder; step 2, adding non-metal powder to inorganic acid, and reacting at 70-110°C for 12-120 hours; step 3, filtering , collect the filtrate, and adjust the pH value; Step 4, add organic aldehyde to the filtrate, heat and stir to prepare solid acetal; Step 5, wash the solid acetal with lye and deionized water to obtain pure solid acetal. The method of the present invention directly synthesizes the epoxy resin in the filtrate into solid acetal, the epoxy resin can be separated from the solution by simple filtration, and the solid acetal with higher added value is obtained, and the recovery of the epoxy resin by the extraction method is avoided The organic solvent used saves cost and is friendly to the environment.

Description

technical field [0001] The invention relates to the technical field of recycling epoxy resin in thermosetting epoxy resin waste, in particular to a solid acetal and a preparation method thereof. Background technique [0002] Epoxy resin is widely used in many fields, such as electronic appliances, electric power industry, wind power generation, chemical industry, aerospace, civil construction, sporting goods, etc. Thermosetting epoxy resin products, commonly known as glass fiber reinforced plastics, are insoluble and infusible due to their special three-dimensional network structure, which makes it difficult to recycle their waste by conventional plastic recycling methods. A large amount of thermosetting epoxy resin waste is piled up in a corner or directly landfilled because it is difficult to recycle. [0003] Typical thermosetting epoxy resin products mainly include printed circuit boards in the electrical and electronic industries, insulating tubes in transformers in th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/56C07C43/303C07C43/307
CPCC07C41/56C07C43/303C07C43/307
Inventor 管传金殷国成
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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