CN106436440A - Fiber forming control production method for poly-m-phenyleneisophthalamide precipitation fiber - Google Patents

Fiber forming control production method for poly-m-phenyleneisophthalamide precipitation fiber Download PDF

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Publication number
CN106436440A
CN106436440A CN201610885719.7A CN201610885719A CN106436440A CN 106436440 A CN106436440 A CN 106436440A CN 201610885719 A CN201610885719 A CN 201610885719A CN 106436440 A CN106436440 A CN 106436440A
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fiber
resin
solidification
meta
solution
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CN106436440B (en
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冷枫
谢静
张鸥
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Sichuan Huiteng Technology Co Ltd
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Sichuan Huiteng Technology Co Ltd
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
    • D21H13/10—Organic non-cellulose fibres
    • D21H13/20—Organic non-cellulose fibres from macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H13/26—Polyamides; Polyimides
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21G—CALENDERS; ACCESSORIES FOR PAPER-MAKING MACHINES
    • D21G1/00—Calenders; Smoothing apparatus

Abstract

The invention discloses a fiber forming control production method for a poly-m-phenyleneisophthalamide precipitation fiber. The method comprises the following steps: 1) adding N,N-dimethylacetamide into a dilution kettle of a poly-m-phenyleneisophthalamide resin solution to form a poly-m-phenyleneisophthalamide resin diluted solution; 2) adding N,N-dimethylacetamide, water, chlorate and mixed alcohol into a solidification liquid to form a resin solidification liquid; 3) blending the resin solidification liquid with the resin diluted solution, respectively conveying the resin solidification liquid and the diluted resin solution into a feed port of a fiber precipitation machine, joining, dispersing and shearing in the precipitation machine to form a precipitation fiber suspension liquid, and overflowing into a solidification barrel; and 4) standing after entering the solidification barrel to promote even growth of a fiber crystal and stable membranous and lamellar morphology. The performance indexes of a product are as follows: the fiber dimension is 0.2-5 mm, the specific surface area is 10-30 m<2>/g, the intrinsic viscosity is 1.6-2.2 dL/g, the absolute dry rate is less than or equal to 15%, the original beating degree is 35-50 OSR, the hot-shrinkage rate at the temperature of 240 DEG C is less than or equal to 20%, and the number of dry pulps is less than or equal to 15 every 6.3 g. The characteristic index of the fiber is changed by controlling the process parameter of the fiber forming process, the development requirements on improvement of product quality or index customized production are met, the technology is advanced, and the one-pass yield of the product and the production effectiveness are greatly improved.

Description

The fiberizing control production method of meta-aramid fibre fibrid
Technical field
The present invention relates to the fiberizing control production of technical field of macromolecules, specially a kind of meta-aramid fibre fibrid Method.
Background technology
It is aqueous cotton-shaped that meta-aramid fibre fibrid characterizes feature, is a kind of fire resistant special type fibre of high comprehensive performance Dimension, with performances such as excellent heat stability, anti-flammability, electrical insulating property, chemical stability, radiation resistances, in manufacture electric insulation The aspects such as paper, high-temperature-resistant filtering material, cellular structural material have extensive the army and the people's purposes.
The production method of fibrid be by meta-aramid amide stock solution and a certain proportion of under stable lower temperature Precipitating solvent delivery mixes to precipitating equipment, and precipitating equipment is operated according to command speed, and stock solution is while shear action is subject to Solidification forms membranaceous or lamellar superbhort fiber, and the fiber of molding has tiny, easy wire-dividing broom purification, and specific surface area is big, the pole on surface Property group many, the features such as easily dispersion in water.
The characteristic index of fibrid includes：Distribution of sizes, beating degree, water retention value, specific surface area, form, wet strong, molecule Amount distribution and degree of crystallinity etc., there is no national standard at present, increase with the purposes of rapidoprint based on fibrid and The downstream product range of application that develops is expanded, it is proposed that the development of quality lifting or index propertiess customized production becomes Gesture, domestic original Technology and precipitating equipment performance are many based on the presence or absence of the domestic fibrid product of solution problem, work Skill regulating measure and equipment performance are not perfect enough, and the shearing force of the such as precipitating equipment output of conventional fixed rotating speed does not have for quantitative Adjustability, the viscosity B coefficent of resin stock solution then transmits the change for fibre morphology and then beating degree, not the receiving of fiber formation process Control, can not meet the growth requirement of product quality lifting or index propertiess customized production.
Existing settling mode (as patent No. ZL201210170766.5) is added before fibrid suspension filtration washing Dress pressure filtration sieve does not meet the inclined crude fibre of size quality requirement to separate in advance, but through physically screening, the one of product Secondary yield can decline, and the faulty fiber for concurrently separating out separately need to be disposed, unfavorable cost control.Therefore improvement is improved existing Technology and equipment performance, by adjusting precipitation machine shearing force, solidification formula of liquid, resin solution proportioning, processing medium temperature Carry out, Deng fiber formation process technological parameter, the precipitating fibre that improving product quality or selectivity production different product quality index are required Dimension product, be for more preferable settling mode.
Content of the invention
The present invention is exactly directed to above technical problem, provides a kind of fiberizing control production of meta-aramid fibre fibrid Method.The method changes the distribution of sizes of fiber, beating degree, water retention value, specific surface by controlling forming process technological parameter The characteristic index such as product, form, wet strong, molecular weight distribution and degree of crystallinity, can meet product quality lifting or index propertiesizations are fixed The growth requirement of system production, compares physics screening mode, advanced technology, and yield of product and productivity effect are greatly improved, city Field competitiveness is significantly improved.
The technical scheme is that：
The fiberizing control production method of meta-aramid fibre fibrid, comprises the following steps：
(1) in the dilution kettle for containing meta-aramid resin solution into DMAC (N, N- dimethylacetamide is allocated by a certain percentage Amine), stir to form meta-aramid resins dilute solution, while regulating and controlling solution temperature by the jacket water (J.W.) of the dilution kettle.Virtue The intrinsic viscosity of synthetic fibre resin solution：1.6～2.2dL/g；The resin concentration of resins dilute solution is calculated as 2%～20% with wt%, 10 DEG C～80 DEG C of temperature.
(2) N,N-dimethylacetamide, water, chlorate, mixed alcohol are allocated into in solidification liquid configuration kettle, stirs to be formed Resin gel solid-liquid, while regulate and control solution temperature by the jacket water (J.W.) of the configuration kettle.Resin gel solid-liquid concentration is calculated as with wt%：DMAC 40%～60%, chlorate 0.1%～5%, mixed alcohol 0.1%～5%, water 30%～50%；Hardening of resin liquid temp controls： 10 DEG C～80 DEG C.Chlorate refers to one or two the mixture in lithium chloride, Sodium Chloride, calcium chloride；Mixed alcohol refer to ethylene glycol, One or two mixture in glycerol.
(3) select the toothed disc multistage-combination series of precipitation machine, select rotating speed, the hardening of resin that will obtain in step (2) The resins dilute solution for obtaining in liquid and step (1) successively delivers into the charging of fiber precipitation machine respectively through flowrate proportioning control Mouthful, crossing in precipitation machine spreads and fibrid suspension is formed after toothed disc shearing, overflow enters to solidify bucket.Resins dilute Liquid inventory and hardening of resin flow quantity proportioning：1：5～60；Precipitation machine toothed disc multistage-combination series：1～5 grade；Precipitation machine turns Speed：1000～9000 revs/min；
(4) fiber crystallisation solidification：Fibrous suspension stands 0.5～2.0h/ batch after stopping entering solidification bucket, promotes fiber Crystalline growth is uniform, and membranaceous and lamellar morphology is stable；
(5) performance indications of fibrid product：0.2～5mm of fiber size；10～30/g of specific surface area；Characteristic is glued Degree：1.6～2.2dL/g；Over dry rate≤15%；35～50 ° of SR of original beating degree；240 DEG C of percent thermal shrinkage≤20%；Dry pulp subnumber ≤ 15/6.3g.
Compared with prior art, beneficial effects of the present invention are：
Change the distribution of sizes of fiber, beating degree, water retention value, specific surface by controlling fiber formation process technological parameter The characteristic index such as product, form, wet strong, molecular weight distribution and degree of crystallinity, can meet product quality lifting or index propertiesizations are fixed The growth requirement of system production, compares physics screening mode, advanced technology, and yield of product and productivity effect are greatly improved, city Field competitiveness is significantly improved.
Description of the drawings
Fig. 1 is that the technological process of the fiberizing control production method of heretofore described meta-aramid fibre fibrid is illustrated Figure.
Specific embodiment
In order that the content of the invention in the present invention easily facilitates understanding, below in conjunction with the drawings and specific embodiments to this Production method described in invention is further elaborated.But this scope for being interpreted as the above-mentioned theme of the present invention should not be only limitted to Following embodiments.
Embodiment 1：
(1) 15～20wt% of resin content, DMAC (N, the N- of the meta-aramid resin of intrinsic viscosity >=1.80dL/g are prepared Dimethyl acetylamide) solution 200Kg；
(2) DMAC being allocated into in the dilution kettle for containing meta-aramid resin solution, stir, configures resin content 6.0 The meta-aramid resins dilute solution of～8.0wt%, regulates and controls 10 DEG C～80 DEG C of solution temperature by diluting the jacket water (J.W.) of kettle；
(3) DMAC, water, lithium chloride, ethylene glycol are allocated into in solidification liquid configuration kettle, stir resin gel solid-liquid is formed, Wt% is calculated as：DMAC 40～60%, LiCl 3%, ethylene glycol 3%, water 30～50%；By configuring kettle Jacket water (J.W.) regulates and controls 10 DEG C～80 DEG C of solution temperature；
(4) 3 grades of built-up gear disks of precipitation machine are selected, 8000 revs/min of rotating speed is selected, by the hardening of resin in step (3) Resins dilute solution in liquid and step (1) is 30 by flow-rate ratio:1 control, successively delivers into the charging of fiber precipitation machine respectively Mouthful, the fibrid suspension of formation, overflow enters to solidify bucket；
(5) fiber crystallisation solidification：Suspension stands 60 minutes after stopping entering solidification bucket；
The fibrid suspension for being obtained by 1 production method of embodiment, after filtration washing, product physical and chemical index is：Fine Dimension size：0.2～5mm；Specific surface area >=25/g；Intrinsic viscosity：1.80dL/g；Over dry rate≤12%；Original beating degree >= 50°SR；240 DEG C of percent thermal shrinkage≤20%；Dry pulp subnumber≤15/6.3g.
Embodiment 2：
(1) 15～20wt% of resin content, DMAC (N, the N- of the meta-aramid resin of intrinsic viscosity >=1.80dL/g are prepared Dimethyl acetylamide) solution 200Kg；
(2) DMAC being allocated into in the dilution kettle for containing meta-aramid resin solution, stir, configures resin content 6.0 The meta-aramid resins dilute solution of～8.0wt%, regulates and controls 10 DEG C～80 DEG C of solution temperature by diluting the jacket water (J.W.) of kettle；
(3) DMAC, water, lithium chloride, ethylene glycol are allocated into in solidification liquid configuration kettle, stir resin gel solid-liquid is formed, Wt% is calculated as with 100%：DMAC 40～60%, LiCl 3%, ethylene glycol 3%, water 30～50%；By configuring the chuck of kettle Water regulates and controls 10 DEG C～80 DEG C of solution temperature；
(4) 3 grades of built-up gear disks of precipitation machine are selected, 6000 revs/min of rotating speed is selected, by the hardening of resin in step (3) Resins dilute solution in liquid and step (1) presses flow 20:1 control, successively delivers into fiber precipitating machine inlet, shape respectively The fibrid suspension for becoming, overflow enters to solidify bucket；
(5) fiber crystallisation solidification：Suspension stands 60 minutes after stopping entering solidification bucket；
The fibrid suspension for being obtained by 1 production method of embodiment, after filtration washing, product physical and chemical index is：Fine Dimension size：0.2～5mm；Specific surface area >=20/g；Intrinsic viscosity：1.80dL/g；Over dry rate≤13%；Original beating degree >= 45°SR；240 DEG C of percent thermal shrinkage≤20%；Dry pulp subnumber≤15/6.3g.
Embodiment 3：
(1) 15～20wt% of resin content, DMAC (N, the N- of the meta-aramid resin of intrinsic viscosity >=1.80dL/g are prepared Dimethyl acetylamide) solution 200Kg；
(2) DMAC being allocated into in the dilution kettle for containing meta-aramid resin solution, stir, configures resin content 6.0 The meta-aramid resins dilute solution of～8.0wt%, regulates and controls 10 DEG C～80 DEG C of solution temperature by diluting the jacket water (J.W.) of kettle；
(3) DMAC, water, lithium chloride, ethylene glycol are allocated into in solidification liquid configuration kettle, stir resin gel solid-liquid is formed, Wt% is calculated as：DMAC 40～60%, LiCl 3%, ethylene glycol 3%, water 30～50%；Molten by the jacket water (J.W.) regulation and control for configuring kettle 10 DEG C～80 DEG C of liquid temp；
(4) 2 grades of built-up gear disks of precipitation machine are selected, 3000 revs/min of rotating speed is selected, by the hardening of resin in step (3) Resins dilute solution in liquid and step (1) presses volume flow 10:1 control, successively delivers into the charging of fiber precipitation machine respectively Mouthful, the fibrid suspension of formation, overflow enters to solidify bucket；
(5) fiber crystallisation solidification：Suspension stands 60 minutes after stopping entering solidification bucket；
The fibrid suspension for being obtained by 3 production method of embodiment, wherein contains fibrid product volume 32.00kg (butt), after filtration washing, product physical and chemical index is：Fiber size：1～5mm；Specific surface area >=10/g；Characteristic Viscosity：1.80dL/g；Over dry rate≤15%；Original beating degree >=35 ° SR；240 DEG C of percent thermal shrinkage≤20%；Dry pulp subnumber≤15 Individual/6.3g.
Embodiment 4：
(1) 15～20wt% of resin content, DMAC (N, the N- of the meta-aramid resin of intrinsic viscosity >=1.80dL/g are prepared Dimethyl acetylamide) solution 200Kg；
(2) DMAC being allocated into in the dilution kettle for containing meta-aramid resin solution, stir, configures resin content 6.0 The meta-aramid resins dilute solution of～8.0wt%, regulates and controls 10 DEG C～80 DEG C of solution temperature by diluting the jacket water (J.W.) of kettle；
(3) DMAC, water, lithium chloride, ethylene glycol are allocated into in solidification liquid configuration kettle, stir resin gel solid-liquid is formed, Wt% is calculated as：DMAC 40～60%, LiCl 5%, ethylene glycol 5%, water 30～50%；Molten by the jacket water (J.W.) regulation and control for configuring kettle 10 DEG C～80 DEG C of liquid temp；
(4) select 1 grade of toothed disc of precipitation machine, select 1000 revs/min of rotating speed, by the resin gel solid-liquid in step (3) and Resins dilute solution in step (1) presses volume flow 50:1 control, successively delivers into fiber precipitating machine inlet, shape respectively The fibrid suspension for becoming, overflow enters to solidify bucket；
(5) fiber crystallisation solidification：Suspension stands 60 minutes after stopping entering solidification bucket；
The fibrid suspension for being obtained by 4 production method of embodiment, after filtration washing, product physical and chemical index is：Fine Dimension size：Fiber size：1～5mm；Specific surface area >=10/g；Intrinsic viscosity：1.80dL/g；Over dry rate≤15%；Original beat The degree of beating >=35 ° SR；240 DEG C of percent thermal shrinkage≤20%；Dry pulp subnumber≤15/6.3g.
The technological parameter of 1～4 production method of embodiment and the part index number comparison sheet of fibrid product
Embodiment 1, embodiment 2 are compared with embodiment 3 and show, by regulating and controlling solidification liquid and dilution liquid flow ratio, precipitating The fibrid product that the technological parameters such as machine rotating speed are obtained has different specific surface areas, beating degree, over dry rate etc., properties of product Index falls progressively；Also indicate that and can change the performance indications of fiber by controlling fiber formation process technological parameter, meet different Product quality requirement or the requirement of index propertiess customized production, controllable advanced technology；Embodiment 4 is compared with embodiment 3 Show, by adjusting process parameter, increase solidification liquid and resin flow ratio extends resin diffusion time, improve chlorate and mixed The wt% content for closing alcohol reduces resin expansion calculation speed, reduces rotating speed and can also produce acquisition same quality product, but in actual work During industry metaplasia is produced, solidification liquid and resin flow ratio are bigger, and economic benefit is poorer.

Claims (5)

1. the fiberizing of meta-aramid fibre fibrid controls production method, it is characterised in that comprise the following steps：
（1）N,N-dimethylacetamide is allocated into in the dilution kettle for containing meta-aramid resin solution by a certain percentage, and stirring is equal Even formation meta-aramid resins dilute solution, while regulate and control solution temperature by the jacket water (J.W.) of the dilution kettle；
（2）N,N-dimethylacetamide, water, lithium chloride, mixed alcohol are allocated into in solidification liquid configuration kettle, stir to form tree Fat solidification liquid, while regulate and control solution temperature by the jacket water (J.W.) of the configuration kettle；
（3）Select the toothed disc combination series of precipitation machine, rotating speed selected, by step（2）In the resin gel solid-liquid that obtains and step （1）In the resins dilute solution that obtains through flowrate proportioning control, successively deliver into fiber precipitating machine inlet respectively, in precipitating Crossing in machine and spreading and fibrid suspension is formed after toothed disc shearing, overflow enters to solidify bucket；
（4）Fiber crystallisation solidification：Suspension is stood after stopping entering solidification bucket, promotes fiber crystalline growth uniform, membranaceous and piece Shape form stable；
（5）The performance indications of fibrid product
Fiber size：0.2～5mm；10～30/g of specific surface area；Intrinsic viscosity：1.6～2.2dL/g；Over dry rate≤15%；Former Beginning beating degree 35～50OSR；240 DEG C of percent thermal shrinkage≤20%；Dry pulp subnumber≤15/6.3g.
2. the fiberizing of meta-aramid fibre fibrid controls production method according to claim 1, it is characterised in that：Resin 1.6～the 2.2dL/g of intrinsic viscosity of solution；The resin concentration of resins dilute solution is calculated as 2～20%, temperature 10 DEG C～80 with w% ℃.
3. the fiberizing of meta-aramid fibre fibrid controls production method according to claim 1, it is characterised in that resin Solidification liquid concentration is calculated as with w%：DMAC 40%～60%, chlorate 0.1%～5%, mixed alcohol 0.1%～5%, water 30%～50%； Chlorate refers to one or two the mixture in lithium chloride, Sodium Chloride, calcium chloride, and mixed alcohol refers in ethylene glycol, glycerol One or two mixture；Solidification liquid temperature control：10 DEG C～80 DEG C.
4. the fiberizing of meta-aramid fibre fibrid controls production method according to claim 1, it is characterised in that resin Dilute solution flow and hardening of resin flow quantity proportioning： 1：5～60；Select precipitation machine toothed disc multistage-combination series：1～5 Level；Select precipitation machine rotating speed：1000～9000 revs/min.
5. the fiberizing of meta-aramid fibre fibrid controls production method according to claim 1, it is characterised in that：Fiber Crystallisation solidification time of repose controls：0.5～2.0h/ batch.
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN110079884A (en) * 2019-05-08 2019-08-02 东华大学 A kind of preparation method of high-specific surface area polyimides fibrid
CN110229350A (en) * 2019-06-21 2019-09-13 赣州龙邦材料科技有限公司 A kind of aramid fiber fibrid and preparation method thereof
CN114481680A (en) * 2022-03-10 2022-05-13 咸宁优维科技有限公司 Preparation method of aramid fiber material and superfine meta-position and para-position aramid fiber film, sponge and aerogel material prepared by same

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CN102373639A (en) * 2010-08-09 2012-03-14 烟台氨纶集团有限公司 Recycling method of waste aramid paper
CN102660795A (en) * 2012-05-29 2012-09-12 四川力通复合材料科技有限公司 Production method of meta-position aramid paper fibrid
CN104630924A (en) * 2015-01-12 2015-05-20 烟台泰和新材料股份有限公司 Method for preparing aromatic polyamide membrane type fibrid

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* Cited by examiner, † Cited by third party
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WO2005059247A1 (en) * 2003-12-09 2005-06-30 Teijin Twaron B.V. Para-aramid fibrid film
CN102373639A (en) * 2010-08-09 2012-03-14 烟台氨纶集团有限公司 Recycling method of waste aramid paper
CN102660795A (en) * 2012-05-29 2012-09-12 四川力通复合材料科技有限公司 Production method of meta-position aramid paper fibrid
CN104630924A (en) * 2015-01-12 2015-05-20 烟台泰和新材料股份有限公司 Method for preparing aromatic polyamide membrane type fibrid

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110079884A (en) * 2019-05-08 2019-08-02 东华大学 A kind of preparation method of high-specific surface area polyimides fibrid
CN110079884B (en) * 2019-05-08 2021-11-02 东华大学 Preparation method of polyimide fibrid with high specific surface area
CN110229350A (en) * 2019-06-21 2019-09-13 赣州龙邦材料科技有限公司 A kind of aramid fiber fibrid and preparation method thereof
CN114481680A (en) * 2022-03-10 2022-05-13 咸宁优维科技有限公司 Preparation method of aramid fiber material and superfine meta-position and para-position aramid fiber film, sponge and aerogel material prepared by same
CN114481680B (en) * 2022-03-10 2023-08-22 咸宁优维科技有限公司 Preparation method of aramid fiber material, aerogel and pumping filter membrane material

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