A polysilazane with excellent spinning performance and its preparation and melt spinning

A polysilazane and melt-spinning technology, which is applied in melt-spinning, textiles and papermaking, single-component synthetic polymer rayon, etc., can solve the problems of complex polymerization device, high polymerization temperature and high cracking temperature, and achieve The preparation process is simple, the polymerization device is simple, and the preparation process is mature.

Active Publication Date: 2022-03-22
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymerization temperature of this method is 300-480°C, and the thermal polymerization reaction is carried out in a pyrolysis column. The pyrolysis temperature is high and the molecular structure is difficult to control.
[0004] It can be found that the following problems exist in the field of polysilazane fiber preparation at present: an activator or catalyst needs to be added during the polymerization process, which increases the difficulty of controlling the degree of polymerization, and at the same time, it is easy to introduce heterogeneous elements and reduce the purity of the product; the polymerization temperature is too high during the polymerization process , the polymerization time is too long, resulting in low polymerization efficiency and increased polymerization cost; the polymerization device is complicated, and a high-temperature cracking column is required, which greatly increases the polymerization cost and the complexity of the preparation process
There are defects in the structure of polysilazane, which leads to the high brittleness of the prepared polysilazane fiber and cannot be wound

Method used

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  • A polysilazane with excellent spinning performance and its preparation and melt spinning
  • A polysilazane with excellent spinning performance and its preparation and melt spinning
  • A polysilazane with excellent spinning performance and its preparation and melt spinning

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Step a: Add 4000ml normal hexane, 503g (4.4mol) methylhydrogen dichlorosilane and 297g ( 2.3mol) dimethyldichlorosilane, N 2 After replacing the air in the bottle, feed NH at a flow rate of 100ml / min 3 , Stir at 0°C for 20h. After the reaction, filter the by-product NH of the ammonolysis reaction4 Cl, fractional distillation of n-hexane to obtain figure 1 700 g of the shown colorless, transparent, oily silazane oligomer with very low viscosity.

[0041] Step b: Add the silazane oligomer prepared in step a into a 500ml three-neck flask, and pass nitrogen gas for 30min after the addition is completed, and the nitrogen flow rate is 50ml / min to ensure that the oxygen in the device is completely exhausted. Stepwise polymerization is adopted, and the heating program is set: 150°C, 0.5h, 200°C, 0.5h, 250°C, 1h, 300°C, 1h, 330°C, 4h. A colorless solid thermoplastic polysilazane was prepared as figure 2 shown.

[0042] The prepared polysilazane and silazane oligomer infra...

Embodiment 2

[0045] Step a: Add 4000ml of normal hexane, 482g (4.2mol) methylhydrogen dichlorosilane and 318g ( 2.5mol) dimethyldichlorosilane, N 2 After replacing the air in the bottle, feed NH at a flow rate of 100ml / min 3 , Stir at 0°C for 20h. After the reaction, filter the by-product NH of the ammonolysis reaction 4 Cl, fractional distillation of n-hexane to obtain a colorless, transparent, oily silazane oligomer with low viscosity.

[0046] Step b and step c are the same as shown in Example 1.

Embodiment 3

[0048] Step a: Add 4000ml of normal hexane, 457g (4.0mol) methylhydrogen dichlorosilane and 343g ( 2.7mol) dimethyldichlorosilane, N 2 After replacing the air in the bottle, feed NH at a flow rate of 100ml / min 3 , Stir at 0°C for 20h. After the reaction, filter the by-product NH of the ammonolysis reaction 4 Cl, fractional distillation of n-hexane to obtain a colorless, transparent, oily silazane oligomer with low viscosity.

[0049] Step b and step c are the same as shown in Example 1.

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Abstract

The invention discloses a polysilazane with excellent spinning performance and its preparation and melt spinning. The main chain of the polysilazane prepared in the present invention is a line-ring structure including a four-membered ring and a six-membered ring. The preparation process includes: component optimization of oligomers prepared by ammonolysis reaction method, stepwise thermal polymerization of oligomers and Melt spinning; the molar ratio of the reaction raw materials is 1:1-1.9:1 methylhydrogendichlorosilane and dimethyldichlorosilane, the reaction solvent is n-hexane, and the volume ratio of n-hexane and raw materials is 4:1 , the silazane oligomer was obtained through ammonolysis reaction, and the polysilazane precursor with excellent spinning performance was obtained through the gradual thermal polymerization of the oligomer; under the condition of 90-120°C, polysilazane was realized by melt spinning Continuous spinning of alkane fibers. The polymerization device of the invention is simple, no external activator is needed in the polymerization process, the reaction process is easy to control, the molecular structure of the prepared polysilazane can be designed, the spinning performance is excellent, and low-temperature melt spinning of continuous fibers can be realized.

Description

technical field [0001] The invention belongs to the field of fiber preparation, and in particular relates to a polysilazane with excellent spinning performance and its preparation and melt spinning. Background technique [0002] Silicon nitride ceramic fibers have excellent properties such as high melting point, good high-temperature mechanical properties, small thermal expansion coefficient, good dielectric properties, low density, and strong oxidation resistance, and have broad application prospects in the field of ceramic matrix composites. Precursor conversion method is the main preparation method of silicon nitride ceramic fiber. The preparation of polysilazane precursors with excellent structural properties and spinning performance is one of the keys to the precursor conversion method, and has attracted the attention of researchers at home and abroad. [0003] Patent CN 104817701A discloses a thermoplastic polysilazane prepared by using methylhydrogendichlorosilane an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/62D01F6/74D01F9/10D01D5/08C04B35/584C04B35/622
CPCC08G77/62D01F6/74D01F9/10D01D5/08C04B35/584C04B35/62295
Inventor 陈建军考可辰李海龙
Owner ZHEJIANG SCI-TECH UNIV
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