Method for utilizing low intermediate phase content asphalt stock to perform continuous spinning to prepare high-quality intermediate phase asphalt precursor fiber

A technology of mesophase and pitch, applied in the field of spinning, can solve the problems of high production cost, complex process, high equipment safety requirements, etc., and achieve the effects of improving the utilization rate, solving broken filaments and reducing the preparation cost.

Active Publication Date: 2017-12-19
上海高强高模新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst used in this method is highly toxic and requires high equipment safety, and solvent dissolution, centrifugation and other processes are still required afterwards. The process is relatively complicated and the production cost is high.
[0006] The preparation process of high-purity mesophase pitch is generally relatively complicated and the production cost is high. Moreover, based on equipment, raw materials and process problems, it is always inevitable to produce pitch with low mesophase content. However, the spinning methods in the prior art only Suitable for high-purity mesophase bitumen raw materials, while these low-mesophase content bitumen cannot be utilized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This example provides a method for preparing high-quality mesophase pitch raw silk by direct spinning of pitch with low mesophase content, including the following steps:

[0036] Step 1: take petroleum pitch with a softening point of 230° C. as the spinning raw material, and determine with a microscope that the mesophase content is 65%.

[0037] Step 2: Get 200g of petroleum asphalt raw material (the quality of the mesophase in the raw material asphalt is 130g), join in the stirring tank;

[0038] Step 3: pressurize the nitrogen to 3.0MPa, stir and heat to 330°C to fully melt the bitumen.

[0039] Step 4: Stop stirring, maintain the pressure at 3.0MPa, the temperature at 330°C, and let stand for 20 minutes.

[0040] Step 5: Slowly release the pressure and vacuumize for 10 minutes, then lower the temperature to 300°C.

[0041] Step 6: Infuse nitrogen again to make the pressure reach 0.3MPa, open the lower valve, and the asphalt enters the spinning machine through the m...

Embodiment 2

[0045] This example provides a method for preparing high-quality mesophase pitch raw silk by direct spinning of pitch with low mesophase content, including the following steps:

[0046] Step 1: Take petroleum pitch with a softening point of 248° C. as the spinning raw material, and determine that the mesophase content is 80%.

[0047]Step 2: Take 100g of petroleum asphalt raw material (the mass of the mesophase in the raw asphalt is 80g), and add it into the stirring tank.

[0048] Step 3: pressurize the nitrogen to 4.0MPa, stir and heat to 355°C to fully melt the bitumen.

[0049] Step 4: Stop stirring, maintain pressure at 4.0MPa, temperature at 355°C, and let stand for 30min.

[0050] Step 5: Slowly release the pressure and vacuumize for 10 minutes, then lower the temperature to 330°C.

[0051] Step 6: Infuse nitrogen again to make the pressure reach 0.3MPa, open the lower valve, and the asphalt enters the spinning machine through the metering pump, so that the asphalt is...

Embodiment 3

[0055] This example provides a method for preparing high-quality mesophase pitch raw silk by direct spinning of pitch with low mesophase content, including the following steps:

[0056] Step 1: Take petroleum pitch with a softening point of 240° C. as the spinning raw material, and determine that the mesophase content is 55%.

[0057] Step 2: Take 300g of petroleum asphalt raw material (the mass of the mesophase in the raw asphalt is 165g), and add it to the stirring tank.

[0058] Step 3: pressurize the nitrogen to 3.0MPa, stir and heat to 340°C to fully melt the bitumen.

[0059] Step 4: Stop stirring, maintain the pressure at 3.0MPa, the temperature at 340°C, and let stand for 15 minutes.

[0060] Step 5: Slowly release the pressure and vacuumize for 10 minutes, then lower the temperature to 315°C.

[0061] Step 6: Inflate nitrogen again to make the pressure reach 0.2MPa, open the lower valve, and the asphalt enters the spinning machine through the metering pump, so that ...

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Abstract

The invention relates to a method for efficiently utilizing low intermediate phase content asphalt to perform direct spinning to prepare high-quality intermediate phase asphalt precursor fiber. According to the method, the low intermediate phase content asphalt is adopted as a raw material, and the method comprises the steps: (1) determining the specific content of an intermediate phase; (2) adding the asphalt to a stirring tank, pressurizing with inert gas, and performing stirring and heating, to fully melt the asphalt; (3) after the asphalt is fully melted, stopping stirring and standing, so as to sink the intermediate phase of the asphalt to the lower portion of melt; (4) depressurizing and vacuumizing to remove bubbles in the molten asphalt; (5) cooling the molten asphalt to a spinning temperature, pressurizing with an inert gas, and switching on a valve to cause the asphalt on the lower portion to enter a spinning machine through a metering pump for spinning, and stopping spinning when the weight of the spun asphalt precursor fiber is lower than or equal to the weight of the intermediate phase in the raw material. According to the method, the utilization rate of the asphalt with the low intermediate phase content can be greatly improved, and the intermediate phase preparation cost and the cost of high-performance pitch-based carbon fiber are reduced.

Description

technical field [0001] The invention relates to the technical field of spinning, in particular to a continuous spinning method for pitch with low mesophase content. Background technique [0002] The raw material heavy oil (aromatic oil, pure compound or other raw materials) is under high temperature and high pressure, and as the reaction proceeds, its aromatic hydrocarbon small molecules gradually aggregate into flat macromolecules, and these molecules are arranged in an orderly manner under the guidance of intermolecular forces. It shows optical anisotropy under the optical polarizing microscope, and people are accustomed to call this region the mesophase, and the pitch containing the mesophase is called the mesophase pitch. [0003] The pitch mesophase exhibits excellent deformability in a certain temperature range, and can maintain a highly ordered arrangement under the extrusion of the spinning pores. This property makes the mesophase pitch have good spinning performance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01D1/04D01D1/09D01D1/10D01D5/08D01F9/00
CPCD01D1/04D01D1/09D01D1/103D01D5/08D01F9/00
Inventor 庞守德查凌迟刘怀成
Owner 上海高强高模新材料科技有限公司
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