Method for reclaiming organosilicon low boiler conversion catalyst

A catalyst and low boiler technology, applied in the field of comprehensive treatment of organosilicon by-products, can solve problems such as volatile acid gas, and achieve the effects of eliminating high activity, simple operation, and eliminating potential safety hazards.

Active Publication Date: 2021-10-22
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the deficiencies in the prior art, the purpose of the present invention is to provide a method for recycling organic silicon low boiler conversion catalysts, which is scientific and reasonable, simple and easy to implement, can completely eliminate the activity of the bottom of the reaction kettle, and solve the problem of volatile acid gas in the bottom of the kettle. problems, eliminate potential safety hazards, and make the recycling process green and environmentally friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 100g of the bottom of the tank after conversion of organic silicon low boilers into the reaction kettle, then carry out hydrolysis reaction with 50g of tap water at 30°C, and equilibrate for 2h; stop the reaction, let it stand for stratification, and the upper layer is a yellow solid-liquid mixed oil phase , the lower layer is the acidic water phase, and the acidic water phase is recovered for use. At 30°C, continuously add 50% sodium hydroxide solution to the yellow solid-liquid mixed oil phase, and keep stirring at a speed of 400r / min until the yellow solid disappears. Add sodium hydroxide solution and continue to stir for 1 h; stand to separate layers, the upper transparent oil phase is recovered for the preparation of glass glue, and the lower layer is saline solution. Under the stirring condition of 400r / min, the brine solution was added dropwise to the recovered acid water until no white precipitate appeared, and the white precipitate was obtained by filtration...

Embodiment 2

[0026] Add 100g of the still bottom after conversion of organic silicon low boilers into the reaction kettle, and then carry out hydrolysis reaction with 60g of industrial water at 40°C, equilibrate for 5h, stop the reaction, let it stand for stratification, and the upper layer is a yellow solid-liquid mixture The oil phase, the lower layer is the acidic water phase, the acidic water phase is recovered for use, and the sodium hydroxide solution with a concentration of 45% is continuously added to the yellow solid-liquid mixed oil phase at 30°C, and kept stirring at a speed of 400r / min until the yellow solid disappears stop adding the sodium hydroxide solution, continue to stir for 3 hours, leave to stand for stratification, the upper transparent oil phase is recovered for the preparation of glass glue, and the lower layer is a saline solution; under the stirring condition of 400r / min, the saline solution is added dropwise to the recovered acid water until the white precipitate ...

Embodiment 3

[0028] Add 100g of the still bottom after conversion of organic silicon low boilers into the reaction kettle, and then carry out hydrolysis reaction with 100g of industrial water at 50°C, equilibrate for 4h, stop the reaction, let it stand for stratification, and the upper layer is a yellow solid-liquid mixture The oil phase, the lower layer is the acid water phase. The acidic water phase is recovered for use, continuously add 40% potassium hydroxide solution to the yellow solid-liquid mixed oil phase at 30°C, and keep stirring at a speed of 400r / min until the yellow solid disappears, stop adding potassium hydroxide solution, and continue stirring After standing for 2 hours, the layers were separated, the upper transparent oil phase was recovered and used for the preparation of glass glue, and the lower layer was saline solution. Under the condition of stirring at 400r / min, the saline solution was added dropwise into the industrial hydrochloric acid solution with a mass ratio ...

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Abstract

The invention belongs to the field of comprehensive treatment of organosilicon by-products, and in particular relates to a method for recovering an organosilicon low boiler conversion catalyst. The recovery method includes the following steps: 1. Add the residual mixture after conversion of organic silicon low boilers into the reaction kettle, add water, and carry out the hydrolysis reaction. After the reaction, leave to stand for stratification, and the upper layer is a yellow solid-liquid mixture. The oil phase, the lower layer is the acidic water phase; add a strong alkali solution to the yellow solid-liquid mixed oil phase at 2.30°C, stir at a speed of 400r / min, stop adding the strong alkali solution until the yellow solid disappears, let stand and separate, and the upper layer is transparent Oil phase, the lower layer is brine solution; 3. Under the condition of 400r / min stirring, add brine solution dropwise to acid water, stop adding brine dropwise when no white precipitate appears, filter to obtain white precipitate, and realize catalyst recovery. The recycling method is simple and easy, can completely eliminate the activity of the bottom of the reaction kettle, and the recycling process is green and environment-friendly.

Description

technical field [0001] The invention belongs to the field of comprehensive treatment of organosilicon by-products, and in particular relates to a method for recovering an organosilicon low boiler conversion catalyst. Background technique [0002] Silicone monomer production enterprises will produce a large number of by-products in the monomer production process, such as high boiling substances, low boiling substances, etc. These byproducts adopt different post-treatment processes due to their own structural characteristics. Organosilicon by-products such as low boilers, azeotropes, etc. undergo disproportionation reactions to achieve group rearrangement, and prepare chlorosilane monomers with more stable structures such as dimethyldichlorosilane. Separate the generated monomers, etc., and the remaining mixture is the bottom of the still. The bottom of the still contains a large amount of conversion catalysts and silicon-chloride bonded substances, which have high activity. E...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B9/02B01J27/32B01J38/48B01J38/64B01J38/60
CPCB01J27/32B01J38/48B01J38/60B01J38/64C01B9/02Y02P20/584
Inventor 伊港蔡水兵胡庆超李云杰国建强孙江
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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