CN102242408A - High-fibrillated polyacrylonitrile (PAN) pulp manufactured by spinning of water-plasticized melt colloid - Google Patents
High-fibrillated polyacrylonitrile (PAN) pulp manufactured by spinning of water-plasticized melt colloid Download PDFInfo
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- CN102242408A CN102242408A CN2010101746711A CN201010174671A CN102242408A CN 102242408 A CN102242408 A CN 102242408A CN 2010101746711 A CN2010101746711 A CN 2010101746711A CN 201010174671 A CN201010174671 A CN 201010174671A CN 102242408 A CN102242408 A CN 102242408A
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- polyacrylonitrile
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Abstract
The invention relates to high-fibrillated polyacrylonitrile (PAN) pulp manufactured by spinning of water-plasticized melt colloid, and in particular relates to a manufacturing method of high-fibrillated PAN pulp. In the method, according to the characteristic that PAN can perform water-plasticized melt operation by means of hydration thereof, PAN powder is fully molten under hydration condition by utilizing a two-stage double screw extruder set, and then the PAN melt spinning colloid is formed at properly reduced temperature; as the colloid is easily oriented under the action of shear force, high shear stress is exerted on the extruder head for high-shear spinning of the colloid so as to form PAN fiber containing rich micro-fiber; and after the obtained fiber is cut off, the cut fiber and water enter grinding equipment at the same time for continuous pulping to finally obtain the high-fibrillated PAN pulp with large specific surface area (up to over 15m<2>/g).
Description
Technical field
The present invention relates to a kind of manufacture method of height primary fibrosis polypropylene nitrile pulp.
Background technology
Polyacryl-nitrile dissolving pulp removes has that polyacrylonitrile itself had: excellent environmental adaptability outside the insensitive and higher serviceability temperature of humidity, also has original fiber degree height, the dispersive property in matrix and reaches dried, as to wet good processability characteristics well.Can replace asbestos or Fanglun slurry cake in most cases and be used for a plurality of fields such as friction sealed material, speciality paper, nonwoven fabric, cost performance is higher.At present, the manufacturing technology aspect finding report of polyacryl-nitrile dissolving pulp is few, and mainly contain following several: blend wet spinning polishing, centrifugal spinning and plasticising melt extrude polishing and precipitation method etc.
Shanghai Lanbang Industry Fibre Co., Ltd. proposes to adopt two kinds of polyacrylonitrile condensates that contain different proportion homogenous configuration monomer to carry out the blend wet spinning at CN200610025775.X, CN200710038948.6, micron-scale phase separation takes place in its mixed slurries in process of setting, form outward appearance and be tantamount to the general fibre tow and the profuse polyacrylonitrile tow of inner fento, after this tow cut-out, staple fiber and water deliver into and pump into milling apparatus simultaneously, under the effect of high-rate of shear, make specific area at 5～15m
2The height primary fibrosis polypropylene nitrile dissolving pulp-like fibre of/g.
USP5296286 has proposed the jet spinning legal system and has been equipped with polyacryl-nitrile dissolving pulp, promptly be that the spinning solution of polyacrylonitrile is extruded by a long slit shape die orifice, stretch or around slit shape mould product, have the high velocity air spray orifice through the high rapid-result airflow apparatus of jet pipe type, stoste extrudes once die orifice, be subjected to the winding-up of high velocity air on every side immediately, thereby form pulp.This method equipment complexity, cost is higher.
Document such as US5401576, KR9208998 has proposed plasticising and has melt extruded polishing and prepare polyacryl-nitrile dissolving pulp, is about to the polyacrylonitrile intensification molten condition of water plasticising, cools to then below the fusing point, makes it become the sloppy heat body; Extrude the back and grind beating, obtaining length is that 1～20mm, diameter are the polyacryl-nitrile dissolving pulp of 0.1～50 μ m.
Proposed among the CN200410093262 to prepare polyacryl-nitrile dissolving pulp with precipitation method, be about to the dissolving fully in dimethylacetylamide isopolarity organic solvent of polyacrylonitrile powder, be mixed with uniform slurries, these slurries inject solidification liquid, under the effect of strong shearing force, directly separate out polyacryl-nitrile dissolving pulp.This method has been omitted operations such as spinning, cut-out, grinding, can reduce manufacturing cost significantly, but these method process conditions are relatively harsher, difficult control.
Summary of the invention
The invention provides a kind of method of making height primary fibrosis polypropylene nitrile pulp.
Technical scheme of the present invention is: utilize polyacrylonitrile to have aquation, can carry out the characteristics of water plasticising fusion, adopt two rank double screw extruder group, make the polyacrylonitrile powder under aquation fully after the fusion, under the condition that suitably reduces temperature, form polyacrylonitrile melt spinning colloid, this colloid is highly susceptible to orientation under the effect of shearing force, apply shearing force at extruder head it is carried out the high shear spinning, form the profuse polyacrylonitrile fibre of inner fento, after the cut-out, enter milling apparatus simultaneously with water, slurrying continuously obtains specific area and is higher than 15m
2The height fibrillation polyacryl-nitrile dissolving pulp of/g.
The present invention compares with existing technology of preparing and has the following advantages:
1. fully profit has the waste silk of polyacrylonitrile fibre, is processed into height primary fibrosis polypropylene nitrile pulp and is used for many high-end products being worth extremely low waste silk, and real the realization turned waste into wealth;
2. utilize water as plasticizer, adopt two rank double screw extruder group that the polyacrylonitrile powder is carried out the spinning of fusion colloid, on the one hand, technological process is simple, environmental protection, economy, on the other hand, water plasticized polypropylene nitrile molten mass is along with the reduction of temperature, the liquid crystal phenomenon of contraposition virtue acid amides spinning slurry can appear in the certain temperature range below fusing point being similar to, at this moment, melt still is single-phase and is very easy to orientation under the effect of shearing force, spinning easily forms the profuse polyacrylonitrile fibre of inner fento under this condition, helps the fiber fibrillation of postorder;
3. the polyacrylonitrile pulp original fiber degree height that makes, specific area is higher than 15m
2/ g.
Description of drawings
Fig. 1 is the process chart of the present invention's height primary fibrosis polypropylene nitrile pulp.
The height primary fibrosis polypropylene nitrile pulp stereoscan photograph that Fig. 2 makes for the inventive method.
The specific embodiment
A kind of method of making height primary fibrosis polypropylene nitrile pulp, utilize polyacrylonitrile to have aquation, can carry out the characteristics of water plasticising fusion, adopt two rank double screw extruder group, make the polyacrylonitrile powder under aquation fully after the fusion, under the condition that suitably reduces temperature, form polyacrylonitrile melt spinning colloid, this colloid is highly susceptible to orientation under the effect of shearing force, apply shearing force at extruder head it is carried out the high shear spinning, form the profuse polyacrylonitrile fibre of inner fento, after the cut-out, enter milling apparatus simultaneously with water, slurrying continuously obtains the height fibrillation polyacryl-nitrile dissolving pulp that specific area is higher than 15m2/g.
Described polyacrylonitrile powder refers to the homopolymer or copolymer of polyacrylonitrile, or conventional polyacrylonitrile waste silk obtains powder through pulverizing.
In the described water plasticized polypropylene nitrile powder, the content of plasticizer water is 10～50wt%, is preferably 15～25wt%.
Described water plasticized polypropylene nitrile melting process is finished on rank on the double screw extruder group, and melt temperature is generally at its more than fusing point 5～40 ℃.
After the complete fusion of described water plasticized polypropylene nitrile, finish on the following rank that are formed on the double screw extruder group of melt spinning colloid, and temperature is generally at its below fusing point 5～30 ℃.
The spinning of described polyacrylonitrile fusion colloid, at the shearing force that cross-head applies, shear rate is 1 * 10
3s
-1～1 * 10
5s
-1.
Described polyacrylonitrile fibre enters milling apparatus with water, simultaneously at 15～45s after cutting off
-1The high-rate of shear effect under, the abundant polyacrylonitrile fibre of inner fento disperses continuously, grinds at aqueous phase, the height fibrillation of realization fiber.
Example 1
Under 100 liters of bands in the kneader of screw rod drawing mechanism, drop into 20 kilogram of 40 purpose polyacrylonitrile waste silk powder, 5 kilograms of deionized waters of spray while mediating, after fully mixing, send into diameter and be Φ 35, draw ratio and be 36, rotating speed is two rank parallel dual-screw extruding machine group of 40 rev/mins, each section temperature of rank extruder is 50 ℃, 160 ℃ and 180 ℃ in the control, make the complete fusion of water plasticized polypropylene nitrile, control each section temperature of rank extruder down is 165 ℃, 150 ℃, 150 ℃, form water plasticized polypropylene nitrile fusion colloid, making the head extrusion pressure simultaneously is 100Kg/cm
2, send into spinning pack after metering, the spinnerets specification is Φ 1.0 * 270 holes, spinning at normal temperatures and pressures, spinning speed is 60m/min, obtains the profuse polyacrylonitrile fibre of inner fento.
Example 2
The polyacrylonitrile fibre of example 1 spinning is cut into 10mm,, feed the charging aperture place simultaneously with the deionized water of the speed of 5kg/h and 500L/h flow and have the disk grinder that promotes impeller, at 40s by cored screw volume type feeding machine
-1The high-rate of shear effect under, the abundant polyacrylonitrile staple fiber of inner fento disperses continuously, grinds at aqueous phase, with the slurries that obtain dewater, after the drying, the polyacryl-nitrile dissolving pulp-like fibre that shredding obtains, distribution of lengths is 2.0 ± 0.4mm, and specific area is 17.8m
2/ g.
Example 3
The polyacrylonitrile of example 1 spinning is cut into 5mm,, feed the charging aperture place simultaneously with the deionized water of the speed of 5kg/h and 200L/h flow and have the disk grinder that promotes impeller, at 40s by cored screw volume type feeding machine
-1High-rate of shear descend, the abundant polyacrylonitrile staple fiber of inner fento disperses continuously, grinds at aqueous phase, with the slurries that obtain dewater, after the drying, the polyacryl-nitrile dissolving pulp-like fibre that shredding obtains, distribution of lengths is 1.8 ± 0.4mm, and specific area is 23.2m
2/ g.
Example 4
The polyacrylonitrile of example 1 spinning is cut into 3mm,, feed the charging aperture place simultaneously with the deionized water of the speed of 5kg/h and 500L/h flow and have the disk grinder that promotes impeller, at 40s by cored screw volume type feeding machine
-1The high-rate of shear effect under, the abundant polyacrylonitrile staple fiber of inner fento disperses continuously, grinds at aqueous phase, with the slurries that obtain dewater, after the drying, the polyacryl-nitrile dissolving pulp-like fibre that shredding obtains, distribution of lengths is 1.6 ± 0.4mm, and specific area is 25.7m
2/ g.
Claims (7)
1. the manufacture method of a height primary fibrosis polypropylene nitrile pulp.It is characterized in that: adopt two rank double screw extruder group, make the polyacrylonitrile powder after abundant fusion under the water plasticization, under the condition that suitably reduces temperature, form polyacrylonitrile melt spinning colloid, this colloid is highly susceptible to orientation under the effect of shearing force, apply shearing force at extruder head it is carried out the high shear spinning, forms the profuse polyacrylonitrile fibre of inner fento, after the cut-out, enter milling apparatus simultaneously with water, slurrying continuously obtains specific area and is higher than 15m
2The height fibrillation polyacryl-nitrile dissolving pulp of/g.
2. the manufacture method of a kind of height primary fibrosis polypropylene nitrile pulp according to claim 1 it is characterized in that described polyacrylonitrile powder refers to the polyacrylonitrile homopolymer or copolymer, or conventional polyacrylonitrile waste silk obtains powder through pulverizing.
3. the manufacture method of a kind of height primary fibrosis polypropylene nitrile pulp according to claim 1 is characterized in that the content of plasticizer water is 10～50wt%, is preferably 15～25wt% in the described water plasticized polypropylene nitrile powder;
4. the manufacture method of a kind of height primary fibrosis polypropylene nitrile pulp according to claim 1 is characterized in that described water plasticized polypropylene nitrile melting process finishes on rank on the double screw extruder group, melt temperature is generally at its more than fusing point 5～40 ℃;
5. the manufacture method of a kind of height primary fibrosis polypropylene nitrile pulp according to claim 1, after it is characterized in that the complete fusion of described water plasticized polypropylene nitrile, finish on the following rank that are formed on the double screw extruder group of melt spinning colloid, and temperature is generally at its below fusing point 5～30 ℃;
6. the manufacture method of a kind of height primary fibrosis polypropylene nitrile pulp according to claim 1 is characterized in that the spinning of described fusion colloid, and at the shearing force that cross-head applies, shear rate is 1 * 10
3s
-1～1 * 10
5s
-1.
7. the manufacture method of a kind of height primary fibrosis polypropylene nitrile pulp according to claim 1, it is characterized in that described cut-out after, promptly enter milling apparatus simultaneously, at 15～45s with water
-1The high-rate of shear effect under, the abundant polyacrylonitrile fibre of inner fento disperses continuously, grinds at aqueous phase, the height fibrillation of realization fiber.
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|---|---|---|---|
| CN2010101746711A CN102242408A (en) | 2010-05-13 | 2010-05-13 | High-fibrillated polyacrylonitrile (PAN) pulp manufactured by spinning of water-plasticized melt colloid |
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|---|---|---|---|
| CN2010101746711A CN102242408A (en) | 2010-05-13 | 2010-05-13 | High-fibrillated polyacrylonitrile (PAN) pulp manufactured by spinning of water-plasticized melt colloid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103437233A (en) * | 2013-09-11 | 2013-12-11 | 顾德芹 | Polyacrylonitrile pulp type fibers as well as preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058896A (en) * | 2006-04-17 | 2007-10-24 | 上海兰邦工业纤维有限公司 | Preparation of polyacrylonitrile pulp-shape fibre |
| CN101280470A (en) * | 2007-04-02 | 2008-10-08 | 上海兰邦工业纤维有限公司 | Method for consciously producing polyacryl-nitrile dissolving pulp-like fibre |
| CN101381898A (en) * | 2008-10-14 | 2009-03-11 | 华南理工大学 | Fibrillation dissolving pulp, method for making same and applications |
-
2010
- 2010-05-13 CN CN2010101746711A patent/CN102242408A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058896A (en) * | 2006-04-17 | 2007-10-24 | 上海兰邦工业纤维有限公司 | Preparation of polyacrylonitrile pulp-shape fibre |
| CN101280470A (en) * | 2007-04-02 | 2008-10-08 | 上海兰邦工业纤维有限公司 | Method for consciously producing polyacryl-nitrile dissolving pulp-like fibre |
| CN101381898A (en) * | 2008-10-14 | 2009-03-11 | 华南理工大学 | Fibrillation dissolving pulp, method for making same and applications |
Non-Patent Citations (1)
| Title |
|---|
| 何翼云等: "聚丙烯腈熔融纺丝技术进展", 《合成纤维工业》, vol. 21, no. 1, 28 February 1998 (1998-02-28), pages 34 - 39 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103437233A (en) * | 2013-09-11 | 2013-12-11 | 顾德芹 | Polyacrylonitrile pulp type fibers as well as preparation method thereof |
| CN103437233B (en) * | 2013-09-11 | 2016-10-05 | 顾德芹 | A kind of polyacryl-nitrile dissolving pulp-like fibre and preparation method thereof |
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Application publication date: 20111116 |