Amino modified silicone oil and preparation method thereof

A technology of amino-modified silicone oil and dihydroxy silicone oil, applied in the direction of carbon fiber, etc., can solve the problems of uneven distribution of groups, easy formation of floating oil on the surface, wide molecular weight distribution of amino-modified silicone oil, etc.

Inactive Publication Date: 2013-09-04
CHINA NAT BLUESTAR (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] There are usually three methods for synthesizing amino silicone oil: 1) D 4 (Octamethylcyclotetrasiloxane) and silane coupling agent are polymerized under catalyst catalysis, but the molecular weight distribution of the amino-modified silicone oil obtained by this method is relatively wide, and the group distribution is not uniform enough; 2) Synthetic ammonia is prepared by emulsion polymerization Based modified silicone emulsion, its disadvantage is that there is a small amount of oligomers in the emulsion, which is easy to form surface floating oil; 3) the linear body is coupled with aminosilane to carry out condensation reaction in the presence of catalyst
However, these methods do not control the metal ion content introduced into the system

Method used

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  • Amino modified silicone oil and preparation method thereof
  • Amino modified silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 30g of dihydroxy silicone oil, 2g of aminosilane coupling agent 602 and 50mg of alkali gel of tetramethylammonium hydroxide to a 100mL three-necked bottle, blow argon gas, and vacuum at low vacuum for 30min. Raise the temperature to 85°C, equilibrate the reaction for 1h under the protection of argon, then slowly start vacuuming, start to control it below -0.02MPa, slowly increase the vacuum degree to -0.09MPa, and vacuumize for 30min; then raise the temperature to 95°C, and stir the reaction 30min; add 0.01mL of n-hexanol, continue to react for 30min; use the same method to vacuumize at -0.09MPa for 1h; release the vacuum, raise the temperature to 165°C under the protection of argon, stir for 1h, destroy the catalyst, and raise the temperature to 200°C to remove the vacuum For small molecules, cool to room temperature. The obtained amino-modified silicone oil had a viscosity of 3750 cSt, and the metal ion content in the product was determined to be 0.021 ppm by ICP....

Embodiment 2

[0036] Add 30g of dihydroxy silicone oil, 2g of aminosilane coupling agent 602 and 36mg of alkali gel of tetramethylammonium hydroxide to a 100mL three-necked bottle, blow argon gas, and evacuate at a low vacuum for 30min. Raise the temperature to 70°C, equilibrate the reaction for 1h under the protection of argon, then slowly start vacuuming, start to control it below -0.02MPa, slowly increase the vacuum degree to -0.09MPa, and vacuumize for 30min; then raise the temperature to 95°C, and stir the reaction 30min; add 0.008mL of octadecylamine, and continue to react for 30min; use the same method to vacuumize at -0.09MPa for 1h; release the vacuum, raise the temperature to 165°C under the protection of argon, stir for 1h, destroy the catalyst, and heat up to 180°C to remove the vacuum. Remove small molecules and cool to room temperature. The obtained amino-modified silicone oil had a viscosity of 2000cSt, and the metal ion content in the product was determined to be 0.022ppm by...

Embodiment 3

[0038] Add 30g of dihydroxysilicone oil and 2g of aminomethyl [N-(3-dimethoxymethylsilyl) propylaminomethyl] propane and alkali glue 100mg of tetramethylammonium hydroxide to a 100mL three-necked bottle , argon blowing, low vacuum vacuum 30min. Raise the temperature to 95°C, equilibrate the reaction for 1 hour under the protection of argon, then slowly start vacuuming, start to control it below -0.02MPa, slowly increase the vacuum degree to -0.09MPa, and vacuumize for 30min; then raise the temperature to 105°C, and stir the reaction 30min; add 0.005mL of hexamethyldisiloxane, and continue to react for 30min; use the same method to vacuumize at -0.09MPa for 1h; release the vacuum, raise the temperature to 165°C under the protection of argon, stir for 1h, destroy the catalyst, and raise the temperature to 200 ℃ to vacuum to remove small molecules, and cooled to room temperature. The obtained amino-modified silicone oil had a viscosity of 8140 cSt, and the metal ion content in t...

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Abstract

The invention relates to amino modified silicone oil which has low content of metal ions and stable viscosity and a preparation method thereof. The amino modified silicone oil is prepared by using dihydroxy silicone oil and an amine coupling agent as raw materials and tetramethylammonium hydroxide as a catalyst, subjecting the above-mentioned materials to a bulk condensation reaction and adding micro-molecular compounds with active groups after the reaction lasts for 2 to 5 h. Compared to conventional methods, the invention has the following characteristics: tetramethylammonium hydroxide is used as a catalyst to substitute metallic compounds, and after the reaction is finished, temperature rises again, which enables the catalyst to be destroyed, the micro-molecular compounds to be removed, the content of metallic impurities in an obtained product of the amino modified silicone oil to be controlled and the amino modified silicone oil with low content of metals and stable viscosity to be synthesized; during utilization, the amino modified silicone oil can substantially reduce metallic impurities introduced into fibers, especially into carbon fiber precursors, thereby improving final quality of carbon fibers, and viscosity of the silicone oil does not change in the process of storage.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to an amino-modified silicone oil with low metal ion content and stable viscosity and a preparation method thereof. Background technique [0002] Carbon fiber has a series of superior characteristics, the most prominent ones are high specific strength and specific modulus. Also has wear resistance, fatigue resistance, creep resistance, chemical inertness and so on. High-quality raw silk is the key to making high-performance carbon fibers. [0003] Since the alkali metal is the oxidation catalyst of carbon, it will promote CO, CO 2 When the gas escapes, some void defects will be left, which will reduce the performance of the carbon fiber; studies have also found that iron ions will also affect the tensile strength and other performance indicators of the original silk fiber. P.Bajaj et al. have studied in detail the reasons for the influence of metal ions on t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/388C08G77/38D06M15/643D06M101/40
Inventor 张希文朱栋栋鲁代仁胡衍平李瑞亢
Owner CHINA NAT BLUESTAR (GRP) CO LTD
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