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A kind of preparation method of lithium polymethylphenylsiloxane alkoxide

A technology of polymethylphenylsiloxane and methylphenyl dialkoxysilane is applied in the field of synthesis of lithium-based compounds, which can solve the problem of phenyl polysiloxane being opaque, affecting appearance, and having few preparation methods. Report and other issues, to achieve the effect of thorough reaction, simple operation and easy availability of raw materials

Active Publication Date: 2018-11-02
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the difference in refractive index, lithium methyl silicon alkoxide will cause phenyl polysiloxane to be opaque during the preparation process and affect the appearance
[0003] In the prior art, the preparation of lithium silicon alkoxide is mostly lithium methyl silicon alkoxide, as in the Chinese patent document CN102491993A (application number 201110378824.9), it is disclosed that N 2 Under the protection, using absolute ethanol, methanol or butanol and cyclohexane as a mixed solvent, lithium hydroxide raw material and hexamethyldisiloxane are used to react lithium trimethylsiliconate, so that the preparation method of lithium siliconate has Great progress has been made, but there are few reports on the preparation method of lithium silanolate containing phenyl

Method used

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  • A kind of preparation method of lithium polymethylphenylsiloxane alkoxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 1000g of methylphenyldiethoxysilane, 50g of lithium hydroxide and 400g of water to a stirring reactor equipped with a rectification tower. Add the rectification column on top, stir the reaction, set the initial temperature to 100°C, and gradually raise the temperature until liquid flows out from the outlet of the rectification tower, and the temperature at the top of the tower is 75°C. When there is no liquid outflow from the outlet of the rectification tower, the second Raise the temperature to 170°C, and liquid flows out again from the outlet of the rectification tower. Keep at 170°C until no liquid flows out from the outlet of the rectification tower. Keep the temperature and vacuumize with nitrogen for 0.5h. The pressure in the reactor is 800Pa. Keep the pressure at 800 Pa with nitrogen, lower the temperature for 2 hours, and cool with nitrogen protection to obtain 665 g of viscous translucent oil, which is lithium polymethylphenylsiloxane.

[0030] After detect...

Embodiment 2

[0032] Add 1000g of methylphenyldimethoxysilane, 35g of lithium hydroxide and 600g of water to a stirring reactor equipped with a rectification tower. Add the rectification column on top, stir the reaction, set the initial temperature to 90°C, and gradually raise the temperature until liquid flows out from the outlet of the rectification tower, and the temperature at the top of the tower is 65°C. When no liquid flows out from the outlet of the rectification tower, the second Raise the temperature to 165°C, and liquid flows out again from the outlet of the rectification tower. Keep at 165°C until no liquid flows out from the outlet of the rectification tower. Keep the temperature and vacuumize with nitrogen for 0.5h. The pressure in the reactor is 1000Pa. Keep the air pressure at 1000 Pa with nitrogen, lower the temperature for 3 hours, and cool under nitrogen protection to obtain 752 g of a viscous translucent oil, which is lithium polymethylphenylsiloxane.

[0033] After dete...

Embodiment 3

[0035] Add 1000g of methylphenyldiethoxysilane, 25g of lithium hydroxide and 800g of water to a stirring reactor equipped with a rectifying tower. The packing of the rectifying tower is a glass spring-type packing. Distillation column, stirring reaction, set the initial temperature to 110°C, and gradually raise the temperature until liquid flows out from the outlet of the rectification tower, and the temperature at the top of the tower is 78°C. ℃, there is liquid outflow from the outlet of the rectification tower, keep 175 ℃ until no liquid flows out from the outlet of the rectification tower, maintain the temperature and pump nitrogen for 0.5h, the pressure in the reaction kettle is 1200Pa, raise the temperature to 230℃ three times, blow nitrogen to maintain the pressure 1200Pa, lowered for 4 hours, nitrogen protection cooling, to obtain 653g of viscous translucent oil, which is lithium polymethylphenylsiloxanate.

[0036] After testing, the yield is 98.6% of the theoretical ...

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Abstract

The invention relates to a preparation method of polypmethyl phenyl siloxane alcohol lithium. The preparation method comprises the following steps: (1) adding methylphenyl dialkoxysilane, lithium hydroxide and water into a reaction kettle of a rectifying column, and stirring to react; (2) carrying out primary heating, controlling the temperature on the top of the rectifying column, reacting until no liquid flows from a discharging hole of the rectifying column, carrying out secondary heating, and reacting until no liquid flows from the discharging hole of the rectifying column; and (3) carrying nitrogen blowing in the reaction kettle, vacuumizing, heating for three time, and cooling by virtue of nitrogen protection, so as to prepare polypmethyl phenyl siloxane alcohol lithium. By virtue of a reactive rectification technique, reactants are continuously removed in the reaction process, so that the reaction is rapid and relatively thorough. The preparation method has the beneficial effects that the raw materials are easily available, the operation is simple, and the postprocessing is avoided.

Description

technical field [0001] The invention relates to a preparation method of lithium polymethylphenylsiloxane alkoxide, which belongs to the technical field of synthesis of lithium compounds. Background technique [0002] The catalysts used in the preparation of polysiloxane by anion catalysis are mainly alkali metal compounds such as sodium, potassium, and lithium hydroxides. Lithium silanolate is a non-equilibrium catalyst. This type of catalyst can only open the ring body at a certain temperature. The silicon-oxygen bond in the linear polysiloxane cannot be cracked, and the Si-O-Si bond in the linear polysiloxane is suitable for the preparation of block polysiloxane or single-end functional group polysiloxane. In the process of making raw rubber or polysiloxane with high phenyl content, when the reaction reaches equilibrium, the reaction system still contains a certain amount of cyclosiloxane, which contains more phenyl groups, and the boiling point High, difficult to remove,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/398
CPCY02P20/10
Inventor 刘海龙许栋伊港张俊朱永和胡庆超王安营刘殿忠张振玉
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL