CN108396581B - Preparation method of fiber pulp and fiber pulp prepared by preparation method - Google Patents
Preparation method of fiber pulp and fiber pulp prepared by preparation method Download PDFInfo
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- CN108396581B CN108396581B CN201810118810.5A CN201810118810A CN108396581B CN 108396581 B CN108396581 B CN 108396581B CN 201810118810 A CN201810118810 A CN 201810118810A CN 108396581 B CN108396581 B CN 108396581B
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- fiber pulp
- pulp
- fiber
- chopped fibers
- pbo
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/20—Methods of refining
- D21D1/34—Other mills or refiners
- D21D1/36—Other mills or refiners with vertical shaft
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
Abstract
The invention relates to the field of preparation of organic fibers, in particular to a preparation method of fiber pulp, which mainly comprises the following steps: and (3) performing mechanical grinding and fibrillation treatment on the chopped fibers through deionized water soaking treatment, liquid nitrogen soaking treatment and a vertical vortex mill in sequence, and separating the chopped fibers from air through a cyclone separator to obtain the fiber pulp. The method has the advantages of stable process, short flow, no pollution to the environment, pure product and no impurity pollution, the average length of the fiber pulp is 0.5-3 mm, and the specific surface area is 6-15 m2The polymer is suitable for the fields of rubber and plastic reinforcement, resin reinforcement, friction materials, sealing materials, high-performance paper and the like.
Description
Technical Field
The invention relates to the field of organic fibers and preparation thereof, in particular to fiber pulp and a preparation method thereof.
Background
The fiber pulp is a differentiated product of fibers, has slightly lower density than the fibers, has the same chemical structure as the fibers, and retains most excellent properties of the fibers. The fiber pulp is in a fluffy shape, rich in hairiness, large in specific surface area and strong in grabbing and binding force with a matrix. Therefore, the fiber pulp has the characteristics of excellent high strength, high modulus, high temperature resistance, flame retardance, wear resistance and the like, and has wide application prospects in the aspects of rubber and plastic reinforcement, resin reinforcement, friction materials, sealing materials, high-performance paper and the like.
In the prior art, the main methods for preparing the fiber pulp are a wet grinding method and a precipitation method. The wet pulp grinding method is to cut the fiber filament into needed length, then to disperse the fiber filament in the specific medium liquid, and to obtain the pulp product through the steps of pulp grinding, pulp screening, filtering, drying, opening and the like. The method has the disadvantages of complex process flow, large amount of wastewater generated in the production process, difficult wastewater treatment and environmental pollution. The precipitation method is that macromolecule liquid crystal state gel formed after the monomer polymerization reaction is injected into a certain solvent, then precipitation is carried out to form precipitation fiber, and the pulp is obtained after washing, drying and opening. Although the precipitation method simplifies the process flow, the polymerization process conditions of the fibers such as PBO fibers, aramid fibers and the like are very harsh, the control difficulty is high, and the stability of the pulp is difficult to ensure.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of fiber pulp, which has the advantages of stable process, short flow, no pollution to the environment, pure product and no impurity pollution,the average length of the fiber pulp is 0.5-3 mm, and the specific surface area is 6-15 m2The polymer is suitable for the fields of rubber and plastic reinforcement, resin reinforcement, friction materials, sealing materials, high-performance paper and the like.
A preparation method of fiber pulp comprises the following steps:
(1) soaking the chopped fibers in water for 10-30min, and controlling the water content to be 30-60%;
(2) soaking the chopped fibers obtained in the step (1) in liquid nitrogen for 5-20 s;
(3) and (3) mechanically grinding and fibrillating the chopped fibers obtained in the step (2) by using a vertical vortex mill, and separating the chopped fibers from air by using a cyclone separator to obtain the fiber pulp.
The length of the chopped fibers in the step (1) is 3-8 mm.
The filament number of the chopped fiber in the step (1) is 1.0D-3.0D, and the elastic modulus is 80-280 GPa.
The chopped fibers in the step (1) comprise one of PBO fibers and aramid fibers.
Preferably, the elastic modulus of the PBO fiber is 180-280 GPa; preferably, the elastic modulus of the aramid fiber is 80-120 GPa.
The rotating speed of the vertical vortex mill is 2000-4000 r/min.
The clearance between the grinding plate of the moving part and the tooth-shaped lining in the vertical vortex mill is 1-3 mm.
The fiber pulp prepared by the method.
The specific surface area of the fiber pulp is 6-15 m2/g。
The average length of the fiber pulp is 0.5-3 mm.
The fiber pulp comprises one of PBO pulp and aramid pulp.
The water used in the present invention is deionized water.
The invention has the beneficial effects that:
(1) after the chopped fibers are soaked in water, the fibril of the fiber core layer is filled with water and fully moisturized; the chopped fibers are quickly treated by adopting low-temperature liquid nitrogen, so that the moisture in the fibers is condensed in situ, and the fibrillation of the chopped fibers is facilitated.
(2) The chopped fibers are mechanically processed by a vertical vortex mill, the chopped fibers are sucked into the bottom of a grinding area by strong attraction generated by rotation of the vertical vortex mill, materials are impacted by a grinding plate rotating at a high speed to obtain kinetic energy under the acceleration of ascending airflow, the materials do high-speed rotation motion under the carrying action of high-speed airflow in a vortex flow field, then the materials centrifugally and tangentially fly out and are impacted by grinding of a tooth-shaped lining, the original direction of the materials is changed after the materials are impacted by the tooth-shaped lining, the materials are impacted by the oncoming grinding plate or the materials moving continuously and annularly, then the materials fly out again and are impacted by the tooth-shaped lining, and the process is repeated. After multiple times of impact action, the material is gradually broken and fibrillated to form the fiber pulp, the fiber pulp enters a separator under the drive of airflow which rises in a vertical vortex mill in a rotating way, and air and the fiber pulp are separated in the separator to prepare pure fiber pulp.
Detailed Description
The present invention and its advantageous effects are described in further detail below with reference to examples, but the embodiments of the present invention are not limited thereto.
Testing method of fiber pulp:
(1) the average fiber length of the fiber pulp is tested according to the standard of GB/T29779-2013 non-polarized light method for measuring the fiber length of the pulp;
(2) the specific surface area of the fiber pulp is tested according to the standard of measuring the specific surface area of a solid substance by GB/T19587-2004 gas adsorption BET method;
example 1
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 3mm, the single-filament fineness of 1.0D and the elastic modulus of 180GPa is soaked in water for 10min, and the water content is controlled to be 30%;
(2) soaking the PBO chopped fibers obtained in the step (1) in liquid nitrogen for 20 s;
(3) and (3) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (2) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 2000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 1mm, and then separating the PBO chopped fibers from air by using a cyclone separator to obtain the PBO pulp.
Example 2
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 8mm, the single-filament fineness of 3.0D and the elastic modulus of 280GPa is soaked in water for 30min, and the water content is controlled to be 60%;
(2) soaking the PBO chopped fibers obtained in the step (1) in liquid nitrogen for 5 s;
(3) and (3) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (2) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 4000r/min, the gap between a grinding plate of a moving part and a tooth-shaped lining in the vertical vortex mill is 3mm, and then separating the PBO chopped fibers from air by using a cyclone separator to obtain the PBO pulp.
Example 3
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 5mm, the filament number of 1.0D and the elastic modulus of 180GPa is soaked in water for 20min, and the water content is controlled to be 40%;
(2) soaking the PBO chopped fibers obtained in the step (1) in liquid nitrogen for 10 s;
(3) and (3) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (2) by a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 4000r/min, the gap between a grinding plate of a moving part and a tooth-shaped lining in the vertical vortex mill is 2mm, and then separating the PBO chopped fibers from air by a cyclone separator to obtain the PBO pulp.
Example 4
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 8mm, the single-filament fineness of 3.0D and the elastic modulus of 280GPa is soaked in water for 10min, and the water content is controlled to be 30%;
(2) soaking the PBO chopped fibers obtained in the step (1) in liquid nitrogen for 5 s;
(3) and (3) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (2) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 2000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 3mm, and then separating the PBO chopped fibers from air by using a cyclone separator to obtain the PBO pulp.
Example 5
The preparation method of the aramid pulp comprises the following steps:
(1) soaking aramid chopped fiber with the length of 3mm, the filament number of 1.0D and the elastic modulus of 80GPa in water for 10min, and controlling the water content to be 30%;
(2) soaking the aramid chopped fibers obtained in the step (1) in liquid nitrogen for 5 s;
(3) and (3) mechanically grinding and fibrillating the aramid chopped fiber obtained in the step (2) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 2000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 1mm, and then separating the aramid chopped fiber from air by using a cyclone separator to prepare the aramid pulp.
Example 6
The preparation method of the aramid pulp comprises the following steps:
(1) soaking aramid chopped fibers with the length of 8mm, the filament number of 3.0D and the elastic modulus of 120GPa in water for 30min, and controlling the water content to be 60%;
(2) soaking the aramid chopped fibers obtained in the step (1) in liquid nitrogen for 20 s;
(3) and (3) mechanically grinding and fibrillating the aramid chopped fibers obtained in the step (2) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 4000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 3mm, and then separating the aramid chopped fibers from air by using a cyclone separator to prepare the aramid pulp.
Comparative examples 1 to 1
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 3mm, the single-filament fineness of 1.0D and the elastic modulus of 180GPa is soaked in liquid nitrogen for 20 s;
(2) and (2) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (1) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 2000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 1mm, and then separating the PBO chopped fibers from air by using a cyclone separator to obtain the PBO pulp.
Comparative examples 1 to 2
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 3mm, the single-filament fineness of 1.0D and the elastic modulus of 180GPa is soaked in water for 10min, and the water content is controlled to be 30%;
(2) and (2) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (1) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 2000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 1mm, and then separating the PBO chopped fibers from air by using a cyclone separator to obtain the PBO pulp.
Comparative examples 1 to 3
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 3mm, the single-filament fineness of 1.0D and the elastic modulus of 180GPa is soaked in water for 10min, and the water content is controlled to be 30%;
(2) soaking the PBO chopped fibers obtained in the step (1) in liquid nitrogen for 20 s;
(3) and (3) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (2) by a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 500r/min, the gap between a grinding plate of a moving part and a tooth-shaped lining in the vertical vortex mill is 5mm, and then separating the PBO chopped fibers from air by a cyclone separator to obtain the PBO pulp.
Comparative examples 1 to 4
A preparation method of PBO pulp comprises the following steps:
(1) PBO chopped fiber with the length of 3mm, the single-filament fineness of 1.0D and the elastic modulus of 180GPa is soaked in water for 10min, and the water content is controlled to be 30%;
(2) soaking the PBO chopped fibers obtained in the step (1) in liquid nitrogen for 20 s;
(3) and (3) mechanically grinding and fibrillating the PBO chopped fibers obtained in the step (2) by using a vertical vortex mill, wherein the rotating speed of the vertical vortex mill is 6000r/min, the gap between a grinding plate of a moving part and a toothed lining in the vertical vortex mill is 0.5mm, and then separating the PBO chopped fibers from air by using a cyclone separator to obtain the PBO pulp.
TABLE 1 Property parameters of the fiber pulps
| Pulp average length (mm) | Specific surface area (m)2/g) | |
| Example 1 | 0.85 | 8.1 |
| Comparative examples 1 to 1 | 2.12 | 1.8 |
| Comparative examples 1 to 2 | 2.58 | 1.5 |
| Comparative examples 1 to 3 | 2.85 | 2.3 |
| Comparative examples 1 to 4 | 0.25 | 12.5 |
| Example 2 | 2.35 | 9.5 |
| Example 3 | 1.64 | 14.2 |
| Example 4 | 2.91 | 6.5 |
| Example 5 | 0.79 | 9.1 |
| Example 6 | 2.96 | 8.5 |
As can be seen from Table 1, the chopped fibers obtained in examples 1 to 6 of the present invention were sequentially subjected to soaking treatment in water, low temperature liquid nitrogen treatment and vertical vortex mill mechanization treatment to obtain fiber pulp having a specific surface area of 6 to 15m2(ii)/g, the average length is 0.5 to 3 mm. When the chopped fibers were not subjected to the immersion treatment in water or the treatment with low-temperature liquid nitrogen as in comparative examples 1-1 and 1-2, the resulting fiber pulp had a very small specific surface area and could not exert the advantage of the pulp during use. When the rotational speed of the vertical vortex mill is too low and the gap between the grinding plate of the moving part and the toothed lining is too large as in comparative examples 1 to 3, the fibrillation force to which the fibers are subjected is small and the prepared pulp is long in length but small in specific surface area of only 2.3m2And/g, the use requirement cannot be met. When the rotating speed of the vertical vortex mill is too high, the grinding plate of the moving part and the tooth-shaped lining are arranged betweenToo small a gap, e.g. comparison
In examples 1 to 4, the chopped fibers were subjected to too small a fibrillation force, the fibers were excessively crushed, and the pulp was too short in length and powdery, and although the specific surface area of the pulp was high, the too small a length of the pulp limited the range of application.
Claims (9)
1. The preparation method of the fiber pulp is characterized by comprising the following steps:
(1) soaking the chopped fibers with the lengths of 3-8 mm in water for 10-30min, and controlling the water content to be 30-60%;
(2) soaking the chopped fibers obtained in the step (1) in liquid nitrogen for 5-20 s;
(3) and (3) mechanically grinding and fibrillating the chopped fibers obtained in the step (2) by using a vertical vortex mill, and separating the chopped fibers from air by using a cyclone separator to obtain the fiber pulp.
2. The method of claim 1, wherein the chopped fibers in step (1) have a single fiber fineness of 1.0D-3.0D and an elastic modulus of 80-280 GPa.
3. The method for producing a fiber pulp according to claim 1, wherein the chopped fibers in the step (1) comprise one of PBO fibers and aramid fibers.
4. The process for producing a fiber pulp according to claim 1, wherein the rotation speed of the vertical vortex mill is 2000 to 4000 r/min.
5. The process for producing a fiber pulp according to claim 1, wherein the clearance between the grinding plate of the moving part and the toothed liner in the vertical vortex mill is 1 to 3 mm.
6. The fiber pulp produced by the method according to any one of claims 1 to 5.
7. The fiber pulp according to claim 6, wherein the specific surface area of the fiber pulp is 6 to 15m2/g。
8. The fiber pulp according to claim 6, wherein the fiber pulp has an average length of 0.5 to 3 mm.
9. The fiber pulp according to claim 7 or 8, wherein the fiber pulp comprises one of a PBO pulp and an aramid pulp.
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| CN201810118810.5A CN108396581B (en) | 2018-02-06 | 2018-02-06 | Preparation method of fiber pulp and fiber pulp prepared by preparation method |
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| CN201810118810.5A CN108396581B (en) | 2018-02-06 | 2018-02-06 | Preparation method of fiber pulp and fiber pulp prepared by preparation method |
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| WO2003020511A1 (en) * | 2001-08-30 | 2003-03-13 | E.I. Du Pont De Nemours And Company | Solid sheet material especially useful for circuit boards |
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| CN103966891A (en) * | 2014-04-23 | 2014-08-06 | 华南理工大学 | Method for preparing fiber pulp and prepared fiber pulp |
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