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Process for preparing alkoxy silicone oligomers

A technology of organosilicon oligomers and alkoxy groups, applied in the field of organosilicon material synthesis, can solve the problems of personnel safety threats, complex reaction process, cumbersome neutralization treatment operation, etc., and achieve stable and easy-to-control reaction process and stable chemical properties , the effect of moderate reactivity

Active Publication Date: 2018-08-03
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The large inventory of by-products and unstable chemical properties pose a great threat to personnel safety, and cause a large amount of ineffective occupation of silicon resources and safety and environmental protection issues. This is an urgent problem facing organic silicon monomer manufacturers.
At present, the treatment method of organosilicon oligomers mainly adopts pyrolysis method to prepare monomers. The disadvantages are that the reaction process is complicated, the selectivity of organosilicon monomers is not high, and the bottoms after pyrolysis are more difficult to handle.
In addition, silicone oligomers are also used to prepare silicone oil, but its disadvantages are that the neutralization treatment of the product is cumbersome, and a large amount of neutralization reagents are used.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Rectify to separate the oligomerization mixture components in the organosilicon by-products, take 500g and put it into a reaction kettle with a rectifying column, then add 500g of toluene, after stirring evenly, add 400g dropwise at 40°C and stirring speed of 400r / min Add methyl ether to the reaction kettle, absorb the generated HCl and use it to prepare hydrochloric acid solution. After the dropwise addition, equilibrate for 5 hours, cool to 30°C, and desorb HCl for 2 hours at 140mmHg, then heat at a speed of 15°C / h by 40 ℃ gradually rises to 70 ℃, and under reduced pressure (under 140mmHg), the low-boiling components in the reacted mixed solution are separated through a rectification column until no liquid is separated, and then 1g of hydrogen carbonate is added to the mixed solution Na, continue stirring for 30 minutes, and filter to obtain a clear neutral alkoxy-substituted organosilicon oligomer, and the product yield can reach 85%.

Embodiment 2

[0043] The oligomer components in the organic silicon by-products were separated by rectification, and 500g was put into a reaction kettle with a rectification column, and then 1000g of cyclohexane was added. After stirring evenly, at 55°C and a stirring speed of 600r / min, Add 600g of diethyl ether to the reaction kettle, the generated HCl is absorbed and used to prepare hydrochloric acid solution, after the dropwise addition is completed, equilibrate for 3h, cool to 25°C, desorb HCl for 1.5h at 100mmHg, and then heat at a speed of 15°C / h Gradually rise from 40°C to 70°C, and under reduced pressure (100mmHg), separate the low-boiling components in the reaction mixture through a rectification column until no liquid is separated, and then add 2g of carbonic acid to the mixture Potassium hydrogen, continuously stirred for 45 minutes, and filtered to obtain a clear neutral alkoxy-substituted organosilicon oligomer, and the product yield can reach 89%.

Embodiment 3

[0045]The oligomer components in the organic silicon by-products were separated by rectification, and 500g was put into a reaction kettle with a rectification column, and then 500g of cyclopentane was added. After stirring evenly, at 65°C and a stirring speed of 700r / min, Add 200g of methanol to the reaction kettle, the generated HCl is absorbed and used to prepare hydrochloric acid solution, after the dropwise addition is completed, equilibrate for 1h, cool to 20°C, and desorb HCl for 1h at 70mmHg, then heat at a speed of 15°C / h by 40 ℃ gradually rises to 70 ℃, under reduced pressure (under 70mmHg), the low-boiling components in the mixed solution after the reaction are separated through a rectification column until no liquid is separated, and then 2.5g of bicarbonate is added to the mixed solution ammonium, continuously stirred for 60 min, and filtered to obtain a clear neutral alkoxy-substituted organosilicon oligomer, and the product yield can reach 92%.

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Abstract

The invention belongs to the field of organosilicon material synthesis and particularly relates to a method for preparing an alkoxyl silicone oligomer. Oligomer components in organic silicon by-products are extracted through distillation, a hydrophobic organic solvent is added to the by-products, then alcohol and ether are added, desorption is performed under reduced pressure after the adding is dropwise completed, low-boiling components are separated out through heating distillation, then a neutralizer is added, and filtration is performed to obtain the alkoxyl silicone oligomer. The alkoxyl silicone oligomer prepared by means of the method is stable in chemical property, safe, environmentally-friendly and easy to store, is an excellent raw material for preparing silicon oil, silicon resin and other organic silicon materials, the problem of production of a large amount of HCl does not exist in the reaction process, and especially the alkoxyl silicone oligomer has an industrial utilization value.

Description

technical field [0001] The invention belongs to the field of organosilicon material synthesis, in particular to a method for preparing alkoxy organosilicon oligomers. Background technique [0002] Oligomers are useful components in the by-products produced during the production of organosilicon monomers. They are mainly mixtures containing silicon-silicon bonds, and are easily hydrolyzed to release a large amount of HCl. The large inventory of by-products and unstable chemical properties pose a great threat to personnel safety, and cause a large amount of ineffective occupation of silicon resources and safety and environmental protection issues. This is an urgent problem faced by organic silicon monomer manufacturers. At present, the treatment method of organosilicon oligomers mainly adopts pyrolysis method to prepare monomers. The disadvantages are that the reaction process is complicated, the selectivity of organosilicon monomers is not high, and the bottoms after pyrolysi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C07F7/20
CPCC07F7/188C07F7/20
Inventor 胡庆超国建强刘德胜宋超周志永周玲张学迪张帅
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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