Unlock instant, AI-driven research and patent intelligence for your innovation.

Intermediate phase asphalt raw material for low-temperature spinning as well as preparation method and application of intermediate phase asphalt raw material

A mesophase pitch and mesophase technology, applied in textiles and papermaking, fiber chemical characteristics, etc., can solve the problems of difficult recovery and recycling of catalysts, decreased fiber strength, and increased carbon fiber manufacturing costs, and achieve long-term stable operation. Narrow distribution, the effect of reducing production costs

Active Publication Date: 2014-12-03
SHANGHAI JIAO TONG UNIV
View PDF5 Cites 9 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solid catalysts such as aluminum trichloride and alumina are difficult to separate from the reaction system, so there is a disadvantage that the catalyst is difficult to recycle and reuse. This not only increases the cost of carbon fiber manufacturing, but the more fatal disadvantage is that even if only a small amount remains in the pitch fiber The catalyst will also lead to a serious decrease in fiber strength in the subsequent pre-oxidation, carbonization, and graphitization projects
Most of the current public information focuses on the development of low softening point asphalt, but there is a lack of research on specific indicators such as the viscosity and molecular weight of qualified spinning solutions and the preparation methods for obtaining these mesophase pitches with qualified indicators.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Methylnaphthalene, hydrogen fluoride and boron trifluoride were added to the reactor at a molar ratio of 1:1.2:0.2. After reacting at 270°C for 120 minutes, nitrogen was continuously fed to remove low-boiling products, and the temperature was lowered to obtain product pitch P1. The reaction yield was 78 wt%. The mesophase content of the product pitch P1 was measured to be 100% by polarizing microscopy.

[0036] The product P1 was dissolved in quinoline with a solubility parameter of 10.7 for 30 minutes, and the insoluble components were separated by filtration to obtain the product pitch P2. The mesophase content of the product pitch P2 was measured to be 60% by polarizing microscopy.

[0037] The product P2 was centrifuged at 320°C for 30 minutes under the protection of nitrogen, and the components with low density in the upper layer were removed after separation to obtain the lower layer product pitch P3. The mesophase content of the product pitch P3 was measured to...

Embodiment 2

[0040] Methylnaphthalene, hydrogen fluoride and boron trifluoride were added to the reactor at a molar ratio of 1:1.2:0.2. After reacting at 270°C for 240 minutes, nitrogen was continuously fed to remove low-boiling products, and the temperature was lowered to obtain the product pitch P1. The reaction yield was 81 wt%. The mesophase content of the product pitch P1 was measured to be 100% by polarizing microscopy.

[0041] The product P1 was treated under the same conditions as in Example 1 to obtain the product pitch P2; the mesophase content of the product pitch P2 was measured to be 60% by polarizing microscopy.

[0042] Then P2 was centrifuged under the same conditions as in Example 1 to obtain product pitch P3. The mesophase content of the product pitch P3 was measured to be 100% by polarizing microscopy. The softening point measured by capillary rheometer is 228°C, the melt viscosity at 270°C measured by rotational rheometer is 48.3Pa·S, and the average molecular weight...

Embodiment 3

[0045] Methylnaphthalene, hydrogen fluoride and boron trifluoride were added to the reactor in a molar ratio of 1:3.0:0.4. After reacting at 270°C for 120 minutes, nitrogen was continuously fed to remove low-boiling products, and the temperature was lowered to obtain the product pitch P1. The reaction yield was 74 wt%. The mesophase content of the product pitch P1 was measured to be 100% by polarizing microscopy.

[0046] The product P1 was treated under the same conditions as in Example 1 to obtain the product pitch P2; the mesophase content of the product pitch P2 was measured to be 60% by polarizing microscopy.

[0047] Then P2 was centrifuged under the same conditions as in Example 1 to obtain product pitch P3. The mesophase content of the product pitch P3 was measured to be 100% by polarizing microscopy. The softening point measured by capillary rheometer is 214°C, the melt viscosity at 270°C measured by rotational rheometer is 40.7 Pa·S, and the average molecular weigh...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
softening pointaaaaaaaaaa
softening pointaaaaaaaaaa
diameteraaaaaaaaaa
Login to View More

Abstract

The invention relates to an intermediate phase asphalt raw material for low-temperature spinning as well as a preparation method and application of the intermediate phase asphalt raw material. The preparation method for the intermediate phase asphalt raw material comprises the following steps: adopting naphthalene-series compounds as raw materials and taking hydrogen fluoride-boron trifluoride as a catalyst to polymerize, dissolving products in heterocyclic aromatic organic solvents with a solubility parameter greater than 10.0, filtering to separate and remove insoluble high-molecular-weight products; then, removing low-molecular-weight products from soluble substances by virtue of a centrifugal separating method, and controlling polymerization conditions and separating conditions of the high-molecular-weight products and the low-molecular-weight products to prepare the intermediate phase asphalt. Compared with the prior art, the intermediate phase asphalt has the characteristics of a low softening point temperature, good melt flowability and narrow molecular weight distribution, can be used for carrying out the spinning at a low temperature lower than 270DEG C, is not only beneficial to long-term stable operation of a spinning process, but also beneficial to lowering the production cost of the intermediate phase asphalt fibers, so that a good solution is provided for producing carbon fibers or other carbon materials with a low cost.

Description

technical field [0001] The invention relates to the field of carbon industry, in particular to a low-temperature spinning mesophase pitch raw material and a preparation method. The mesophase pitch raw material can finally prepare high-strength and high-modulus high-performance pitch-based carbon fibers. Background technique [0002] High-performance carbon fiber is light, has high strength and high elastic modulus, and plays a huge role as a high-value material in the fields of defense industry, aerospace, cutting-edge technology, pillar industry, and daily life. The demand for high-performance carbon fiber is increasing. The rate of more than 10% has increased significantly year by year. [0003] According to the classification of raw materials used, carbon fiber can be divided into polyacrylonitrile-based (PAN) carbon fiber, pitch-based carbon fiber and viscose-based carbon fiber. At present, carbon fiber products are mainly the first two types, of which PAN-based carbon ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/10D01F9/145
Inventor 杨斌王新灵刘媛张媛媛宋晨晨
Owner SHANGHAI JIAO TONG UNIV