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 PDF

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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
pulp
water
pan
colloid
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CN2010101746711A
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尤松
尤秀兰
陈洪新
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上海兰邦工业纤维有限公司
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Publication of CN102242408A publication Critical patent/CN102242408A/en

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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

水增塑熔融胶体纺制高度原纤化聚丙烯腈浆粕 Aqueous colloidal plasticized melt spinning highly fibrillated polyacrylonitrile pulp

技术领域 FIELD

[0001] 本发明涉及一种高度原纤化聚丙烯腈浆粕的制造方法。 [0001] The present invention relates to a method for producing a highly fibrillated polyacrylonitrile pulp. 背景技术 Background technique

[0002] 聚丙烯腈浆粕除具有聚丙烯腈本身所具有的:优异的环境适应性,对湿度不敏感以及较高的使用温度外,还具有原纤化程度高、在基体中的分散性能好及干、湿加工性能好的特点。 [0002] In addition to having polyacrylonitrile polyacrylonitrile pulp itself has: excellent in environmental adaptability, are not sensitive to humidity and high temperature, but also has a high degree of fibrillation, dispersibility in the matrix good and dry, wet processing and good performance. 在绝大多数情况下可以取代石棉或芳纶浆粕用于摩擦密封材料、特种纸、无纺布等多个领域,性价比较高。 In most cases the replacement of asbestos or aramid pulp can be used in various fields of friction sealing materials, specialty paper, nonwoven fabric, the higher cost. 目前,聚丙烯腈浆粕的制造技术方面所见报导不多,主要有以下几种:共混湿法纺丝研磨法、离心纺丝法和增塑熔融挤出研磨法以及沉析法等。 Currently, polyacrylonitrile pulp manufacturing technique aspect seen little reported, are the following: milling a blend wet spinning, centrifugal spinning and melt-extruded plasticized polishing method and precipitation method.

[0003] 上海兰邦工业纤维有限公司在CN200610025775. X、CN200710038948. 6提出采用含有不同比例同种结构单体的两种聚丙烯腈聚合体进行共混湿法纺丝,其混和浆液在凝固过程中发生微观相分离,形成外观无异于普通纤维丝束而内部微纤非常丰富的聚丙烯腈丝束,将该丝束切断后,短切纤维和水同时输送进入和泵入研磨设备,在高剪切速率的作用下,制得比表面积在5〜15m2/g的高度原纤化聚丙烯腈浆粕状纤维。 [0003] Industrial Fiber Co., Ltd. on Hai Lanbang made using two kinds of species containing different proportions of the same structure of the monomer polyacrylonitrile polymer blended wet spinning, which is mixed in the slurry in the solidification process CN200610025775. X, CN200710038948. 6 microphase separation occurs, forming the external appearance is no different from common microfibrillated fiber strands and the interior is very rich polyacrylonitrile tow after the tow cut, chopped fiber and delivered into the water and pumped simultaneously grinding equipment, under the action of high shear rates, made larger than the surface area of ​​the highly fibrillated 5~15m2 / g polyacrylonitrile pulp-shaped fiber.

[0004] USP5296286提出了喷射纺丝法制备聚丙烯腈浆粕,即是将聚丙烯腈的纺丝原液通过一长的狭缝形模口而被挤出,经喷管型的高速成气流装置所拉伸或在狭缝形模品周围开有高速气流喷孔,原液一经模口压出,立即受到周围高速气流的喷吹,从而形成浆粕。 [0004] USP5296286 proposed apparatus polyacrylonitrile pulp jet spinning process, i.e., a polyacrylonitrile spinning dope is extruded through a long slit-shaped die, into a high speed through the nozzle-type air flow means the stretching or slit-shaped die around the high velocity gas stream article injection hole is opened, a liquid pressed out through the die, by blowing immediately around the high velocity gas stream, to form a pulp. 该方法设备复杂,成本较高。 The method apparatus complex and costly.

[0005] US5401576, KR9208998等文献提出了增塑熔融挤出研磨法制备聚丙烯腈浆粕,即将用水增塑的聚丙烯腈升温熔融状态,然后降温到熔点以下,使其成为过冷熔体;挤出后研磨叩解,得到长度为1〜20mm、直径为0. 1〜50μπι的聚丙烯腈浆粕。 [0005] US5401576, KR9208998 other document proposes plasticized melt extrusion triturated Preparation of Poly Method polyacrylonitrile pulp, i.e. water plasticized polyacrylonitrile heated molten state, and then cooled to below the melting point, making it a supercooled melt; grinding beating after extrusion, to give a length of 1~20mm, a diameter of 0. 1~50μπι polyacrylonitrile pulp.

[0006] CN200410093262中提出了用沉析法制备聚丙烯腈浆粕,即将聚丙烯睛粉末在二甲基乙酰胺等极性有机溶剂中完全溶解,配制成均勻的浆液,该浆液注入凝固液中,在强剪切力的作用下,直接沉析出聚丙烯腈浆粕。 [0006] CN200410093262 proposed precipitation with polyethylene prepared by Method polyacrylonitrile pulp, i.e. polyacrylonitrile powder was completely dissolved in dimethyl acetamide polar organic solvent to prepare a homogeneous slurry, the slurry is injected into the coagulating liquid , under the action of strong shear forces, the precipitated directly polyacrylonitrile pulp. 该法省略了纺丝、切断、研磨等工序,可以大幅度降低制造成本,但该方法工艺条件比较苛刻,较难控制。 This method is omitted spinning, cutting, grinding processes, it can greatly reduce the manufacturing cost, but the process conditions are harsh, more difficult to control.

发明内容 SUMMARY

[0007] 本发明提供一种制造高度原纤化聚丙烯腈浆粕的方法。 [0007] The present invention provides a method for producing highly fibrillated polyacrylonitrile pulp.

[0008] 本发明的技术方案是:利用聚丙烯睛具有水合作用,可进行水增塑熔融的特点,采用双阶双螺杆挤出机组,使聚丙烯腈粉末在水合作用下充分熔融后,在适当降低温度的条件下形成聚丙烯腈熔融纺丝胶体,该胶体在剪切力的作用下非常易于取向,在挤出机头施加高剪切应力对其进行高剪切纺丝,形成内部微纤非常丰富的聚丙烯腈纤维,切断后,与水同时进入研磨设备,连续制浆,得到比表面积高于15m2/g的高度原纤维化聚丙烯腈浆粕。 [0008] The aspect of the present invention are: the use of polyacrylonitrile having hydration, the water can be plasticized melt characteristics, dual stage twin-screw extruder unit, polyacrylonitrile powder hydration sufficiently melted in the forming a melt spinning polyacrylonitrile colloid at a temperature appropriate to reduce the effect of shear forces in the colloid is very easy alignment, high shear stress is applied to them in a high shear extruder head spun, formed internal microfibers very rich polyacrylonitrile fiber, after cutting, while the water entering the grinding apparatus, a continuous pulp, highly fibrillated specific surface area above 15m2 / g of polyacrylonitrile pulp.

[0009] 本发明与现有制备技术相比具有以下优点: [0009] The present invention relates to the preparation of the prior art has the following advantages:

[0010] 1.可以充分利有聚丙烯腈纤维的废丝,将价值极低的废丝加工成高度原纤化聚丙烯腈浆粕用于许多高端产品,真正实现变废为宝;[0011] 2.利用水作为增塑剂,采用双阶双螺杆挤出机组对聚丙烯腈粉体进行熔融胶体纺丝,一方面,工艺流程简单、环保、经济,另一方面,水增塑聚丙烯腈熔融体随着温度的降低, 在熔点以下的一定的温度范围内会出现类似于对位芳酰胺纺丝浆液的液晶现象,此时,熔体仍为单相且在剪切力的作用下非常容易取向,在该条件下纺丝易形成内部微纤非常丰富的聚丙烯腈纤维,有利于后序的纤维原纤化; [0010] 1. You can take full advantage of polyacrylonitrile fiber waste silk, silk waste will be processed into low-value highly fibrillated polyacrylonitrile pulp used in many high-end products, truly turning waste into treasure; [0011 ] 2. The use of water as a plasticizer, a dual stage twin screw extruder unit polyacrylonitrile powder was melt-spun colloid, on the one hand, the process is simple, environmentally friendly, economical, on the other hand, water plasticized polypropylene nitrile melt as the temperature decreases, there will be similar to the liquid crystal phenomenon aramid spinning the slurry in a temperature range below the melting point, at this time, still melt and in a single phase shear force is easily oriented in the spinning condition is easy to form a very rich inner microfibers polyacrylonitrile fibers, fibrillated facilitate the subsequent;

[0012] 3.制得的聚丙烯睛浆粕原纤化程度高,比表面积高于15m2/g。 [0012] 3. High polyacrylonitrile pulp obtained degree of fibrillation, a specific surface area greater than 15m2 / g. 附图说明 BRIEF DESCRIPTION

[0013] 图1为本发明高度原纤化聚丙烯腈浆粕的工艺流程图。 [0013] Figure 1 is a process flow diagram of a polyacrylonitrile highly fibrillated pulp invention.

[0014] 图2为本发明方法制造的高度原纤化聚丙烯腈浆粕扫描电镜照片。 [0014] FIG. 2 of the present invention, a method for producing highly fibrillated polyacrylonitrile pulp SEM photograph.

具体实施方式 Detailed ways

[0015] 一种制造高度原纤化聚丙烯腈浆粕的方法,利用聚丙烯腈具有水合作用,可进行水增塑熔融的特点,采用双阶双螺杆挤出机组,使聚丙烯腈粉末在水合作用下充分熔融后, 在适当降低温度的条件下形成聚丙烯腈熔融纺丝胶体,该胶体在剪切力的作用下非常易于取向,在挤出机头施加高剪切应力对其进行高剪切纺丝,形成内部微纤非常丰富的聚丙烯腈纤维,切断后,与水同时进入研磨设备,连续制浆,得到比表面积高于15m2/g的高度原纤维化聚丙烯腈浆粕。 Method [0015] A method for manufacturing a highly fibrillated polyacrylonitrile pulp, using a polyacrylonitrile having hydration, the water can be plasticized melt characteristics, dual stage twin-screw extruder unit, polyacrylonitrile powder after the hydration sufficiently melted to form a melt-spinning polyacrylonitrile colloids under conditions appropriate to reduce the temperature, the colloid is very easy orientation under the action of shearing force, application of high shear stress in the extruder head thereof high shear spun microfibers are formed inside a very rich polyacrylonitrile fiber, after cutting, while the water entering the grinding apparatus, a continuous pulp, a specific surface area above 15m2 / g of highly fibrillated polyacrylonitrile pulp meal.

[0016] 所述的聚丙烯腈粉末指的是聚丙烯腈的均聚体或共聚体,或者是常规聚丙烯腈废丝经粉碎得到粉末。 [0016] The polyacrylonitrile is polyacrylonitrile powder refers to homo- or copolymers, polyacrylonitrile, waste silk or a conventional pulverized to obtain a powder.

[0017] 所述的水增塑聚丙烯腈粉末中,增塑剂水的含量为10〜50wt%,最好为15〜 25wt%。 [0017] The water-plasticized polyacrylonitrile powder, the water content of the plasticizer is 10~50wt%, preferably 15~ 25wt%.

[0018] 所述的水增塑聚丙烯腈熔融过程在双螺杆挤出机组的上阶完成,熔融温度一般在其熔点以上5〜40°C。 [0018] The water-plasticized polyacrylonitrile melting process in order to complete the twin-screw extrusion unit, typically a melting temperature above its melting point 5~40 ° C.

[0019] 所述的水增塑聚丙烯腈完全熔融后,熔融纺丝胶体的形成在双螺杆挤出机组的下阶完成,温度一般在其熔点以下5〜30°C。 [0019] The water-plasticized polyacrylonitrile completely melted to form a molten spun colloid in order to complete a double screw extrusion unit, generally at a temperature below its melting point 5~30 ° C.

[0020] 所述的聚丙烯腈熔融胶体纺丝,在挤出机机头施加的高剪切应力,剪切速率为IX IoV1 〜ι XioV1. [0020] The colloidal melt spinning polyacrylonitrile, high shear stress is applied in the extruder head shear rate IX IoV1 ~ι XioV1.

[0021] 所述的聚丙烯腈纤维切断后,与水同时进入研磨设备,在15〜45s—1的高剪切速率作用下,内部微纤丰富的聚丙烯腈纤维在水相中连续分散、研磨,实现纤维的高度原纤化。 [0021] The polyacrylonitrile fibers after cutting, while the water entering the grinding apparatus, at a high shear rate acting 15~45s-1, the inner microfibers rich polyacrylonitrile fibers dispersed in a continuous aqueous phase, polishing of highly fibrillated fibers.

[0022]实例 1 [0022] Example 1

[0023] 在100升带下螺杆出料装置的捏合机中,投入20公斤40目的聚丙烯腈废丝粉体, 边捏合边喷淋5公斤去离子水,充分混合后,送入直径为Φ35、长径比为36、转速为40转/ 分的双阶同向双螺杆挤出机组,控制上阶挤出机的各段温度为50°C、16(TC和180°C,使水增塑聚丙烯腈完全熔融,控制下阶挤出机的各段温度为165°C、150°C、150°C,形成水增塑聚丙烯腈熔融胶体,同时使机头挤出压力为lOOKg/cm2,经计量后送入喷丝组件,喷丝板规格为Φ 1. 0 X 270孔,在常温常压下纺丝,纺丝速率为60m/min,得到内部微纤非常丰富的聚丙烯腈纤维。 [0023] In 100 liters screw kneader vaginal discharge outlet means, the object 40 into 20 kg polyacrylonitrile waste silk powder while kneading the shower side 5 kg of deionized water, thoroughly mixed, and fed to a diameter of Φ35 an aspect ratio of 36, speed 40 rev / min with a two stage twin screw extrusion unit, to control the temperature of each stage extruder was 50 ° C, 16 (TC and 180 ° C, increasing the water temperature of each plasticized polyacrylonitrile completely melted, under the control stage extruder was 165 ° C, 150 ° C, 150 ° C, the water formed in the molten plasticized polyacrylonitrile colloid, while the pressure of extruded material lOOKg / cm2, was metered into the spin pack to the spinneret specification Φ 1. 0 X 270 holes, under normal temperature and pressure in the spinning, the spinning rate of 60m / min, to give a very rich inner microfiber polyacrylonitrile fiber.

[0024]实例 2 [0024] Example 2

4[0025] 将实例1纺制的聚丙烯腈纤维切断成10mm,通过空心螺杆体积式喂料机,以^g/ h的速率和500L/h流量的去离子水同时喂入进料口处带有推动叶轮的盘式研磨机,在40s—1 的高剪切速率作用下,内部微纤丰富的聚丙烯腈短切纤维在水相中连续分散、研磨,将得到的浆液脱水、干燥后,开松得到的聚丙烯腈浆粕状纤维,长度分布为2. 0士0. 4mm,比表面积为17. 8m2/go 4 [0025] The polyacrylonitrile fiber spun Example 1 was cut into 10mm, through the hollow screw volumetric feeder, deionized water ^ g / h rate and 500L / h feed flow rate while the feed throat after having driven wheel disk mill, at a high shear rate of 40s-1 action, the internal microfibers rich polyacrylonitrile chopped fibers dispersed in a continuous aqueous phase, triturated and the resulting slurry was dehydrated and dried , opening obtained polyacrylonitrile pulp-shaped fiber length distribution of 2.0 disabilities 0. 4mm, the specific surface area was 17. 8m2 / go

[0026]实例 3 [0026] Example 3

[0027] 将实例1纺制的聚丙烯睛纤维切断成5mm,通过空心螺杆体积式喂料机,以^g/h 的速率和200L/h流量的去离子水同时喂入进料口处带有推动叶轮的盘式研磨机,在40s—1 的高剪切速率作下,内部微纤丰富的聚丙烯腈短切纤维在水相中连续分散、研磨,将得到的浆液脱水、干燥后,开松得到的聚丙烯腈浆粕状纤维,长度分布为1.8士0. 4mm,比表面积为23. 2m2/g。 [0027] The polyacrylonitrile fiber spun Example 1 was cut into 5mm, through the hollow screw volumetric feeder, deionized water ^ g / h rate and 200L / h flow rate while feeding with the feed throat there driven impeller disc mill, a high shear rate for at 40s-1, the inner microfibers rich polyacrylonitrile chopped fibers dispersed in a continuous aqueous phase, triturated and the resulting slurry was dehydrated and dried, opening obtained polyacrylonitrile pulp-shaped fiber length distribution of 1.8 disabilities 0. 4mm, the specific surface area was 23. 2m2 / g.

[0028] 实例4 [0028] Example 4

[0029] 将实例1纺制的聚丙烯睛纤维切断成3mm,通过空心螺杆体积式喂料机,以^g/h 的速率和500L/h流量的去离子水同时喂入进料口处带有推动叶轮的盘式研磨机,在40s—1 的高剪切速率作用下,内部微纤丰富的聚丙烯腈短切纤维在水相中连续分散、研磨,将得到的浆液脱水、干燥后,开松得到的聚丙烯腈浆粕状纤维,长度分布为1. 6士0. 4mm,比表面积为25. 7m2/go [0029] The polyacrylonitrile fiber spun Example 1 was cut into 3mm, through the hollow screw volumetric feeder, deionized water ^ g / h rate and 500L / h flow rate while feeding with the feed throat there driven impeller disk mill, at a high shear rate of 40s-1 action, the internal microfibers rich polyacrylonitrile chopped fibers dispersed in a continuous aqueous phase, triturated and the resulting slurry was dehydrated and dried, opening obtained polyacrylonitrile pulp-shaped fiber length distribution of 1.6 disabilities 0. 4mm, the specific surface area was 25. 7m2 / go

Claims (7)

1. 一种高度原纤化聚丙烯腈浆粕的制造方法。 1. A method of manufacturing pulp highly fibrillated polyacrylonitrile. 其特征在于:采用双阶双螺杆挤出机组,使聚丙烯腈粉末在水增塑作用下充分熔融后,在适当降低温度的条件下形成聚丙烯腈熔融纺丝胶体,该胶体在剪切力的作用下非常易于取向,在挤出机头施加高剪切应力对其进行高剪切纺丝,形成内部微纤非常丰富的聚丙烯腈纤维,切断后,与水同时进入研磨设备,连续制浆,得到比表面积高于15m2/g的高度原纤维化聚丙烯腈浆粕。 Characterized in that: a dual stage twin screw extruder unit, polyacrylonitrile powder was sufficiently melted in the plasticizing effect of water, colloid forming polyacrylonitrile melt spinning under conditions appropriate to reduce the temperature, the shearing force in colloid under the action of very easy alignment, high shear stress is applied to them in a high shear extruder head spun microfibers are formed inside a very rich polyacrylonitrile fiber, after cutting, while the water entering the grinding apparatus, a continuous system pulp, highly fibrillated specific surface area above 15m2 / g of polyacrylonitrile pulp.
2.根据权利要求1所述的一种高度原纤化聚丙烯腈浆粕的制造方法,其特征在于所述的聚丙烯腈粉末指的是聚丙烯腈均聚体或共聚体,或者是常规聚丙烯腈废丝经粉碎得到粉末。 2. A highly fibrillated polyacrylonitrile pulp manufacturing method according to claim 1, wherein said polyacrylonitrile is polyacrylonitrile powder refers to homo- or copolymer, or a conventional polyacrylonitrile waste silk was pulverized to obtain a powder.
3.根据权利要求1所述的一种高度原纤化聚丙烯腈浆粕的制造方法,其特征在于所述的水增塑聚丙烯腈粉末中,增塑剂水的含量为10〜50wt%,最好为15〜25wt% ; 3. A highly fibrillated polyacrylonitrile pulp manufacturing method according to claim 1, wherein said water-plasticized polyacrylonitrile powder, the water content of the plasticizer is 10~50wt% , more preferably 15~25wt%;
4.根据权利要求1所述的一种高度原纤化聚丙烯腈浆粕的制造方法,其特征在于所述的水增塑聚丙烯腈熔融过程在双螺杆挤出机组的上阶完成,熔融温度一般在其熔点以上5 〜40°C ; A method for producing a highly fibrillated polyacrylonitrile pulp according to claim 1, wherein said water-plasticized polyacrylonitrile melting process is completed on the order of a twin screw extruder unit, a molten above its melting point temperature is generally 5 ~40 ° C;
5.根据权利要求1所述的一种高度原纤化聚丙烯腈浆粕的制造方法,其特征在于所述的水增塑聚丙烯腈完全熔融后,熔融纺丝胶体的形成在双螺杆挤出机组的下阶完成,温度一般在其熔点以下5〜30°C ; 5. A highly fibrillated polyacrylonitrile pulp manufacturing method according to claim 1, wherein after the water is completely melted plasticized polyacrylonitrile, colloid-forming melt spinning in a twin-screw extrusion the lower-order unit is completed, the temperature is generally below its melting point at 5~30 ° C;
6.根据权利要求1所述的一种高度原纤化聚丙烯腈浆粕的制造方法,其特征在于所述的熔融胶体纺丝,在挤出机机头施加的高剪切应力,剪切速率为IXlO3iT1〜IXio5iT1. A method for producing a highly fibrillated polyacrylonitrile pulp according to claim 1, wherein the melt-spinning of colloidal, high shear stress is applied in the extruder head shear rate IXlO3iT1~IXio5iT1.
7.根据权利要求1所述的一种高度原纤化聚丙烯腈浆粕的制造方法,其特征在于所述的切断后,即与水同时进入研磨设备,在15〜45s—1的高剪切速率作用下,内部微纤丰富的聚丙烯腈纤维在水相中连续分散、研磨,实现纤维的高度原纤化。 7. A highly fibrillated polyacrylonitrile pulp manufacturing method according to claim 1, characterized in that after the cutting, i.e. simultaneously with water into the grinding apparatus, in the high shear of 15~45s-1 under the action of shear rate, internal microfibers rich polyacrylonitrile fibers dispersed in a continuous aqueous phase, polishing of highly fibrillated fibers.
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