CN109338495A - A method of Modal fibre is prepared by raw material of reed straw - Google Patents
A method of Modal fibre is prepared by raw material of reed straw Download PDFInfo
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- CN109338495A CN109338495A CN201811216251.8A CN201811216251A CN109338495A CN 109338495 A CN109338495 A CN 109338495A CN 201811216251 A CN201811216251 A CN 201811216251A CN 109338495 A CN109338495 A CN 109338495A
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- reed straw
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- 239000000835 fiber Substances 0.000 title claims abstract description 227
- 235000014676 Phragmites communis Nutrition 0.000 title claims abstract description 190
- 239000010902 straw Substances 0.000 title claims abstract description 184
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000002994 raw material Substances 0.000 title claims abstract description 25
- 238000009987 spinning Methods 0.000 claims abstract description 81
- 229920002678 cellulose Polymers 0.000 claims abstract description 41
- 239000001913 cellulose Substances 0.000 claims abstract description 41
- 239000000126 substance Substances 0.000 claims abstract description 37
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 230000035800 maturation Effects 0.000 claims abstract description 22
- 238000012545 processing Methods 0.000 claims abstract description 16
- 230000015271 coagulation Effects 0.000 claims abstract description 14
- 238000005345 coagulation Methods 0.000 claims abstract description 14
- 108010059892 Cellulase Proteins 0.000 claims abstract description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 9
- 238000009835 boiling Methods 0.000 claims abstract description 9
- 229940106157 cellulase Drugs 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 9
- 238000007711 solidification Methods 0.000 claims abstract description 9
- 230000008023 solidification Effects 0.000 claims abstract description 9
- 238000004061 bleaching Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 8
- 230000023556 desulfurization Effects 0.000 claims abstract description 8
- 238000005554 pickling Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 136
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 106
- 238000011010 flushing procedure Methods 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 238000007654 immersion Methods 0.000 claims description 31
- 229920000297 Rayon Polymers 0.000 claims description 30
- 239000003292 glue Substances 0.000 claims description 29
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 23
- 239000002518 antifoaming agent Substances 0.000 claims description 21
- 239000012459 cleaning agent Substances 0.000 claims description 21
- 239000003921 oil Substances 0.000 claims description 21
- 239000008399 tap water Substances 0.000 claims description 21
- 235000020679 tap water Nutrition 0.000 claims description 21
- 238000002791 soaking Methods 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 16
- -1 sulphonic acid ester Chemical class 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000012752 auxiliary agent Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 239000007844 bleaching agent Substances 0.000 claims description 13
- 230000001112 coagulating effect Effects 0.000 claims description 13
- 229920003043 Cellulose fiber Polymers 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 9
- 108010029541 Laccase Proteins 0.000 claims description 8
- 239000007832 Na2SO4 Substances 0.000 claims description 8
- 239000004115 Sodium Silicate Substances 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 8
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 8
- 235000010265 sodium sulphite Nutrition 0.000 claims description 8
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 8
- 239000011686 zinc sulphate Substances 0.000 claims description 8
- 108090000790 Enzymes Proteins 0.000 claims description 7
- 102000004190 Enzymes Human genes 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 229940088598 enzyme Drugs 0.000 claims description 7
- 230000032050 esterification Effects 0.000 claims description 7
- 238000005886 esterification reaction Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 239000006260 foam Substances 0.000 claims description 7
- 238000012805 post-processing Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 7
- 239000001814 pectin Substances 0.000 claims description 6
- 229920001277 pectin Polymers 0.000 claims description 6
- 235000010987 pectin Nutrition 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
- 108010059820 Polygalacturonase Proteins 0.000 claims 1
- 238000007598 dipping method Methods 0.000 claims 1
- 108010093305 exopolygalacturonase Proteins 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 description 45
- 230000007935 neutral effect Effects 0.000 description 9
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000012263 liquid product Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004627 regenerated cellulose Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000011094 fiberboard Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
It is the method that raw material prepares Modal fibre the present invention relates to a kind of reed, it is characterized in that obtaining cellulose by techniques such as cleaning, soda boiling, pickling, cellulase treatment and organic solvent processing using reed straw as main raw material(s)；Then it is alkalized to cellulose, is experienced, spinning solution is made in yellow, filtering, the techniques such as defoaming and maturation；Spinning solution solidification forming in spinning coagulation bath obtains nascent strand；Spinneret drawing-off is carried out to nascent strand and obtains fiber, this fiber is defoamed, desulfurization, the obtained Modal fibre of techniques such as bleaching, washes, oil and dry.The dry breaking strength of Modal fibre prepared by the present invention is between 3.4~3.6cN/dtex, and dry elongation at break is between 12%~14%；Its wet breaking strength is between 2.2~2.3cN/dtex, and wet elongation at break is between 14%~15%.Main mechanical properties test shows: Modal fibre prepared by the present invention substantially conforms to the definition according to international chemical standard fibre office (BISFA) to Modal fibre.
Description
Technical field
The invention belongs to Modal fibre technical fields, and in particular to a kind of to prepare Modal fibre by raw material of reed straw
The method of dimension.
Background technique
Modal (Modal) fiber is a kind of regenerated celulose fibre, its chemical composition is cellulose.Modal fibre
It is one kind of koplon, performance is better than common viscose fiber.In recent years, domestic viscose rayon manufacturer is more
Number has all carried out the exploitation of Modal fibre.Modal fibre breaking strength is high, elongation at break is small, hygrometric state modulus is high, and has
Good alkali resistance.Modal fibre is defined in international chemistry standard fibre office (BISFA), is obtained by process
High-intensitive and high wet modulus regenerated cellulose is obtained, wet breaking strength is less than in 2.20cN/dtex or more, wet elongation at break
15%.
Reed is a kind of very strong renewable plant of vitality, is widely cultivated in China.The main component of reed straw
Containing 48~54% cellulose, 18~20% lignin, 12~15% pentosan, 5~8% hemicellulose, 2~
4% ash content etc..The high cellulose content of reed straw provides possibility for its raw material for being used as Modal fibre.
Currently, the primary raw material of Modal fibre is wood pulp cellulose and cotton pulp cellulose, seek a kind of cheap, matter
Reliable fibrous raw material is measured to replace wood pulp and cotton pulp cellulose be significantly.Reed straw is cheap, and it contains
There is a large amount of cellulose, but the comparison of ingredients of reed is complicated, further includes pentosan, lignin and hemicellulose other than cellulose
Element etc..The composition of Modal fibre is cellulose, to obtain high-quality using reed as the Modal fibre of raw material, just must will
The removal such as pentosan, lignin and hemicellulose, otherwise, the quality of fiber will be poor.Reed straw has content of cellulose
High unique advantage is applied in many fields, and such as: Chinese Patent Application No. 201610304352.5 reports a kind of reed
The production method of reed stalk fiber board；Chinese Patent Application No. 201610302005.9 reports a kind of utilization reed straw system
The method of standby cement grinding aid, however, shortcoming is the fibrous plate and cement grinding aid prepared using reed straw as raw material
Added value of product it is not high.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, one kind is provided by raw material of reed straw and prepares Modal fibre
The method of dimension.The present invention extracts cellulose from reed straw, is then prepared as Modal fibre, this Modal fibre tool
The performance of standby excellent spinning material.Low value-added reed straw is prepared as the Modal fibre of added value by the present invention, is answered
With having a extensive future.
A kind of method that Modal fibre is prepared as raw material using reed straw of the present invention, which is characterized in that described
Method comprises the following steps:
(1) clean: dry reed straw saw is broken, saw it is broken after every section length about 2~5cm, by saw it is broken after reed straw
Stalk is cleaned with warm water, and cleaning agent (all-round neutral cleaners, upper sea blue winged fine chemistry industry Science and Technology Ltd. production) is added,
Cleaning agent dosage accounts for the 0.01%~0.05% of reed straw, reed straw quality (g) and cleaning agent aqueous solution volume (mL)
Bath raio is 1 ︰ 100~500, and tap water repeated flushing is used after cleaning；
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 40~60, is added
Enter the sodium hydroxide of 3~6g/L sodium metasilicate, 3~8g/L sodium sulfite and 6~15g/L, kiering temperature is 70 DEG C~80 DEG C, kiering
Time is 100~110min；After kiering, with 35 DEG C~40 DEG C of warm water repeated flushing to neutrality；
(3) pickling: under room temperature, it is 2~4g/L sulfuric acid and 2 that the reed straw that step (2) are handled, which is immersed in mass concentration,
In the mixed solution of~3g/L hydrochloric acid, bath raio is 1 ︰ 40~50, and soaking time is 30~50min；After immersion, with 30 DEG C~
40 DEG C of warm water repeated flushing is to neutrality；
(4) cellulase treatment: under room temperature, it is 2~4g/L fruit that the reed straw that step (3) are handled, which is immersed in mass concentration,
In glue enzyme solutions, control pH value is 6~7.5, and temperature is 55 DEG C~65 DEG C, and soaking time is 2~4h, and bath raio is 1 ︰ 35~55；
After immersion, it is in 2~3g/L laccase solution that reed straw, which is immersed in mass concentration, and control pH value is 6.5~7.5, temperature
It is 55 DEG C~65 DEG C, soaking time is 3~4h, and bath raio is 1 ︰ 40~50；After immersion, with tap water repeated flushing into
Property；
(5) organic solvent is handled: the reed straw that step (4) are handled being immersed in ethanol solution, temperature control is 45
DEG C~60 DEG C, it is stirred continuously, mixing time is 2~4h；After stirring, filtering removes filtrate, and remaining solid flocculent substance is
For cellulose fibre, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw in air
Cellulose；
(6) alkalization of reed straw pulp fibers element: treated that reed straw cellulose is dissolved in 10 by step (5)~
20g/L NaOH solution, is added the auxiliary agent JL-EBZ of Accessories during Binzhou Ju Li Chemical Co., Ltd. production, and auxiliary agent JL-EBZ accounts for reed straw
The mass values of stalk pulp are 0.4~1.5%, and dip time is 4~5 hours, 1 ︰ 5~8 of bath raio；
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into always
Forming apparatus, controlled at 12~18 DEG C, ageing time is 5~6 hours；
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2
Reaction, CS2Volume (mL) and reed straw pulp fibers element quality (g) than being 1 ︰ 120~150, the reaction time for 1.5~
3 hours, reaction temperature was 60~80 DEG C；The NaOH that concentration is 50~100g/L is added in cellulose sulfonate after yellow is reacted
The volume ratio of solution dissolution, cellulose sulfonate and NaOH solution is 1 ︰ 2~4；
(9) filtering and defoaming of viscose glue: by step (8) treated reed straw pulp fibers element sulphonic acid ester using filtering
Machine filtering；Filtered viscose glue is removed the bubble in reed straw pulp fibers element sulphonic acid ester using continuously and rapidly defoaming method
It removes, obtains viscose glue；
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 8~
20 DEG C, the time is 5~8 hours, must reach the spinning solution for spinning Modal fibre, wherein the esterification degree of spinning solution is
65~75；
(11) the poly- limited public affairs of power chemical industry in Accessories during Binzhou the preparation before spinning: are added in step (10) treated spinning solution
The spin bath additive JL-FS of production is taken charge of, additional amount is the 0.15~0.25% of bath foam volume；Then it is public that letter Anda, Changzhou is added
The defoaming agent CD-FFA01 of production is taken charge of, the additional amount of defoaming agent is the 0.02~0.15% of spinning solution volume；Wherein, spinning solution
Viscosity be 100~120Pas；
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath,
Coagulating bath by 70~80g/L H2SO4, 70~90g/L ZnSO4, 80~150g/L Na2SO4, remaining is water, solidifies bath temperature
Degree is 35~50 DEG C, and spinning speed is 35~50m/min, and Immersion time of the strand in coagulating bath is 0.8~2 second；
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand carries out spinneret drawing-off, this
Method is negative drawing-off, and degree of draft is -40%~-60%, and plasticizing drawing-off is 110%~135%, and the drawing-off that bounces back after drawing-off is -
1%~-4%；
(14) it is molten that step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent that concentration is 0.2~1.5g/L
Liquid (model: XS-K660A, Xu Shi Chemical Industry Science Co., Ltd production), immersing the time is 0.5~1 hour, and solution temperature is normal
Temperature, 1 ︰ 15~20 of bath raio；
(15) desulfurization of fiber: step (14) treated fiber is immersed into the NaOH solution that concentration is 3~4g/L, is immersed
Time is 2~4 hours, and solution temperature is 75~90 DEG C, 1 ︰ 10~20 of bath raio；
(16) it is molten that step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent that concentration is 0.1~0.5g/L
Liquid (title: bleaching powder, the production of Guangzhou Yue Jia Chemical Industry Science Co., Ltd), immersing the time is 1~3 hour, solution temperature 30
~50 DEG C, 1 ︰ 10~15 of bath raio；
(17) washing of fiber: step (16) treated fiber being immersed in 70~95 DEG C of hot water, and the time is 1~2
Hour, 1 ︰ 10~20 of bath raio；
(18) fiber oils: by the oil bath solution (model: DY- of step (17) treated fiber immerses 4~8g/L
NL1022, the production of Jining Hua Kai resin Co., Ltd), oil bath temperature is 75~85 DEG C, and the time is 1~4 hour, 1 ︰ 10 of bath raio~
20；
(19) drying of fiber: by step (18), treated, and fiber obtains Modal fibre after drying and processing.
The present invention has following distinguishing feature:
(1) present invention does breaking strength between 3.4~3.6cN/ by Modal fibre prepared by raw material of reed straw
Between dtex, dry elongation at break is between 12%~14%；Modal fibre wet breaking strength is between 2.2~2.3cN/
Between dtex, the wet elongation at break of fiber between 14%~15%, the Modal fibre of strength property and buying
Strength property is close.The present invention meets international chemical standard fibre by cellulose fibre prepared by raw material of reed straw substantially
Definition of the office to Modal fibre.
(2) present invention is extracted from reed straw by the methods of soda boiling, acidity, cellulase treatment and organic solvent processing
Cellulose is prepared as Modal fibre, and whole simple production process, production process environmental pollution is small, has promotion price
Value.
(3) reed straw is originally a kind of plant that economic value is low, and the present invention is prepared as Modal fibre, significantly mentions
The high economic value of reed straw.
Specific embodiment
The present invention is described in detail in embodiment described below.
Embodiment 1
(1) clean: weighing 3000 grams of dry reed straw, reed straw is sawed it is broken, saw it is broken after every section length about 2~
3cm, by saw it is broken after reed straw cleaned with warm water, cleaning agent (all-round neutral cleaners, upper sea blue winged fining is added
The production of work Science and Technology Ltd.), cleaning agent dosage accounts for the 0.01% of reed straw, and reed straw quality (g) is water-soluble with cleaning agent
The bath raio of liquid product (mL) is 1 ︰ 100, and tap water repeated flushing is used after cleaning.
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 40, is added
The sodium hydroxide of 3g/L sodium metasilicate, 3g/L sodium sulfite and 6g/L, kiering temperature are 70 DEG C, and the kiering time is 100min.Kiering
After, with 35 DEG C of warm water repeated flushing to neutrality.
(3) pickling: under room temperature, it is 2g/L sulfuric acid and 2g/L that the reed straw that step (2) are handled, which is immersed in mass concentration,
In the mixed solution of hydrochloric acid, bath raio is 1 ︰ 40, soaking time 30min.After immersion, extremely with 40 DEG C of warm water repeated flushing
It is neutral.
(4) cellulase treatment: under room temperature, it is 2g/L pectin that the reed straw that step (3) are handled, which is immersed in mass concentration,
In enzyme solutions, control pH value is 6.5, and temperature is 55 DEG C, soaking time 2h, and bath raio is 1 ︰ 35.After immersion, reed straw
Being immersed in mass concentration is in 2g/L laccase solution, and control pH value is 6.5, and temperature is 55 DEG C, soaking time 3h, and bath raio is 1 ︰
40.After immersion, with tap water repeated flushing to neutrality.
(5) organic solvent is handled: the reed straw that step (4) are handled being immersed in ethanol solution, temperature control is 45
DEG C, it is stirred continuously, mixing time 2h.After stirring, filtering removes filtrate, and remaining solid flocculent substance is cellulose
Fiber, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw cellulose in air.
(6) alkalization of reed straw pulp fibers element: by step (5), treated that reed straw cellulose is dissolved in 10g/L
NaOH solution, is added the auxiliary agent JL-EBZ of Accessories during Binzhou Ju Li Chemical Co., Ltd. production, and auxiliary agent JL-EBZ accounts for reed straw pulp
Mass values be 0.4%, dip time be 4 hours, 1 ︰ 5 of bath raio.
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into always
Forming apparatus, controlled at 12 DEG C, ageing time is 5 hours.
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2
Reaction, CS2Volume (mL) and reed straw pulp fibers element quality (g) than be 1 ︰ 120, the reaction time be 1.5 hours, instead
Answering temperature is 60 DEG C.Cellulose sulfonate after yellow is reacted is added the NaOH solution that concentration is 50g/L and dissolves, cellulose sulphur
The volume ratio of acid esters and NaOH solution is 1 ︰ 2.
(9) filtering and defoaming of viscose glue: by step (8) treated reed straw pulp fibers element sulphonic acid ester using filtering
Machine filtering；Filtered viscose glue is removed the bubble in reed straw pulp fibers element sulphonic acid ester using continuously and rapidly defoaming method
It removes, obtains viscose glue.
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 8 DEG C,
Time is 5 hours, must reach the spinning solution of spinning Modal fibre, wherein the esterification degree of spinning solution is 69.8.
(11) the poly- limited public affairs of power chemical industry in Accessories during Binzhou the preparation before spinning: are added in step (10) treated spinning solution
The spin bath additive JL-FS of production is taken charge of, additional amount is the 0.15% of bath foam volume；Then the production of Changzhou letter AnDa Co., Ltd is added
Defoaming agent CD-FFA01, the additional amount of defoaming agent is the 0.02% of spinning solution volume；Wherein, the viscosity of spinning solution is
115.6Pa·s。
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath,
Coagulating bath by 70g/L H2SO4, 70g/L ZnSO4, 80g/L Na2SO4, remaining is water, and coagulation bath temperature is 50 DEG C, spinning
Speed is 35m/min, and Immersion time of the strand in coagulating bath is 0.8 second.
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand carries out spinneret drawing-off, this
Method is negative drawing-off, and degree of draft is -48.9%, and plasticizing drawing-off is 125%, and the drawing-off that bounces back after drawing-off is -1.5%.
(14) step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent solution (type that concentration is 0.2g/L
Number: the production of XS-K660A, Xu Shi Chemical Industry Science Co., Ltd), immersing the time is 0.5 hour, and solution temperature is room temperature, 1 ︰ of bath raio
15。
(15) desulfurization of fiber: immersing the NaOH solution that concentration is 3g/L for step (14) treated fiber, when immersion
Between be 2 hours, solution temperature be 75 DEG C, 1 ︰ 10 of bath raio.
(16) step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent solution (name that concentration is 0.1g/L
Claim: bleaching powder, the production of Guangzhou Yue Jia Chemical Industry Science Co., Ltd), immersing the time is 1 hour, and solution temperature is 30 DEG C, 1 ︰ of bath raio
10。
(17) washing of fiber: step (16) treated fiber being immersed in 70 DEG C of hot water, and the time is 1 hour, bath
Than 1 ︰ 10.
(18) fiber oils: by the oil bath solution (model: DY-NL of step (17) treated fiber immerses 4g/L
1022, the production of Jining Hua Kai resin Co., Ltd), oil bath temperature is 75 DEG C, and the time is 1 hour, 1 ︰ 10 of bath raio.
(19) drying of fiber: by step (18), treated that fiber obtains Modal fibre a after drying and processing.
Embodiment 2
(1) clean: weighing 3000 grams of dry reed straw, reed straw is sawed it is broken, saw it is broken after every section length about 4~
5cm, by saw it is broken after reed straw cleaned with warm water, cleaning agent (all-round neutral cleaners, upper sea blue winged fining is added
The production of work Science and Technology Ltd.), cleaning agent dosage accounts for the 0.02% of reed straw, and reed straw quality (g) is water-soluble with cleaning agent
The bath raio of liquid product (mL) is 1 ︰ 300, and tap water repeated flushing is used after cleaning.
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 50, is added
The sodium hydroxide of 4g/L sodium metasilicate, 5g/L sodium sulfite and 10g/L, kiering temperature are 75 DEG C, and the kiering time is 105min.Kiering
After, with 35 DEG C of warm water repeated flushing to neutrality.
(3) pickling: under room temperature, it is 3g/L sulfuric acid and 2.5g/ that the reed straw that step (2) are handled, which is immersed in mass concentration,
In the mixed solution of L hydrochloric acid, bath raio is 1 ︰ 45, soaking time 40min.After immersion, with 35 DEG C of warm water repeated flushing
To neutrality.
(4) cellulase treatment: under room temperature, it is 3g/L pectin that the reed straw that step (3) are handled, which is immersed in mass concentration,
In enzyme solutions, control pH value is 6.5, and temperature is 60 DEG C, soaking time 3h, and bath raio is 1 ︰ 50.After immersion, reed straw
Being immersed in mass concentration is in 2.5g/L laccase solution, and control pH value is 7, and temperature is 60 DEG C, soaking time 4h, and bath raio is 1 ︰
50.After immersion, with tap water repeated flushing to neutrality.
(5) organic solvent is handled: the reed straw that step (4) are handled being immersed in ethanol solution, temperature control is 60
DEG C, it is stirred continuously, mixing time 3h.After stirring, filtering removes filtrate, and remaining solid flocculent substance is cellulose
Fiber, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw cellulose in air.
(6) alkalization of reed straw pulp fibers element: by step (5), treated that reed straw cellulose is dissolved in 15g/L
NaOH solution, is added the auxiliary agent JL-EBZ of Accessories during Binzhou Ju Li Chemical Co., Ltd. production, and auxiliary agent JL-EBZ accounts for reed straw pulp
Mass values be 1%, dip time be 4 hours, 1 ︰ 6 of bath raio.
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into always
Forming apparatus, controlled at 15 DEG C, ageing time is 5 hours.
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2
Reaction, CS2Volume (mL) and reed straw pulp fibers element quality (g) than be 1 ︰ 120, the reaction time be 3 hours, react
Temperature is 60~80 DEG C.Cellulose sulfonate after yellow is reacted is added the NaOH solution that concentration is 80g/L and dissolves, cellulose
The volume ratio of sulphonic acid ester and NaOH solution is 1 ︰ 3.
(9) filtering and defoaming of viscose glue: by step (8) treated reed straw pulp fibers element sulphonic acid ester using filtering
Machine filtering；Filtered viscose glue is removed the bubble in reed straw pulp fibers element sulphonic acid ester using continuously and rapidly defoaming method
It removes, obtains viscose glue.
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 15
DEG C, the time is 7 hours, must reach the spinning solution of spinning Modal fibre, wherein the esterification degree of spinning solution is 69.2.
(11) the poly- limited public affairs of power chemical industry in Accessories during Binzhou the preparation before spinning: are added in step (10) treated spinning solution
The spin bath additive JL-FS of production is taken charge of, additional amount is the 0.20% of bath foam volume；Then the production of Changzhou letter AnDa Co., Ltd is added
Defoaming agent CD-FFA01, the additional amount of defoaming agent is the 0.08% of spinning solution volume；Wherein, the viscosity of spinning solution is
110.5Pa·s。
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath,
Coagulating bath by 76g/L H2SO4, 79g/L ZnSO4, 100g/L Na2SO4, remaining is water, and coagulation bath temperature is 50 DEG C, spinning
Speed is 40m/min, and Immersion time of the strand in coagulating bath is 1.5 seconds.
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand carries out spinneret drawing-off, this
Method is negative drawing-off, and degree of draft is -55.9%, and plasticizing drawing-off is 120%, and the drawing-off that bounces back after drawing-off is -1.5%.
(14) step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent solution (type that concentration is 0.6g/L
Number: the production of XS-K660A, Xu Shi Chemical Industry Science Co., Ltd), immersing the time is 0.5 hour, and solution temperature is room temperature, 1 ︰ of bath raio
15。
(15) desulfurization of fiber: immersing the NaOH solution that concentration is 3g/L for step (14) treated fiber, when immersion
Between be 3 hours, solution temperature be 75 DEG C, 1 ︰ 10 of bath raio.
(16) step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent solution (name that concentration is 0.3g/L
Claim: bleaching powder, the production of Guangzhou Yue Jia Chemical Industry Science Co., Ltd), immersing the time is 2 hours, and solution temperature is 40 DEG C, 1 ︰ of bath raio
10。
(17) washing of fiber: step (16) treated fiber being immersed in 90 DEG C of hot water, and the time is 1.5 hours,
1 ︰ 15 of bath raio.
(18) fiber oils: by the oil bath solution (model: DY- of step (17) treated fiber immerses 6g/L
NL1022, the production of Jining Hua Kai resin Co., Ltd), oil bath temperature is 80 DEG C, and the time is 2 hours, 1 ︰ 15 of bath raio.
(19) drying of fiber: by step (18), treated that fiber obtains Modal fibre b after drying and processing.
Embodiment 3
(1) clean: weighing 3000 grams of dry reed straw, reed straw is sawed it is broken, saw it is broken after every section length about 2~
3cm, by saw it is broken after reed straw cleaned with warm water, cleaning agent (all-round neutral cleaners, upper sea blue winged fining is added
The production of work Science and Technology Ltd.), cleaning agent dosage accounts for the 0.03% of reed straw, and reed straw quality (g) is water-soluble with cleaning agent
The bath raio of liquid product (mL) is 1 ︰ 300, and tap water repeated flushing is used after cleaning.
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 50, is added
The sodium hydroxide of 5g/L sodium metasilicate, 6g/L sodium sulfite and 9g/L, kiering temperature are 75 DEG C, and the kiering time is 105min.Kiering
After, with 35 DEG C of warm water repeated flushing to neutrality.
(3) pickling: under room temperature, it is 3g/L sulfuric acid and 2g/L that the reed straw that step (2) are handled, which is immersed in mass concentration,
In the mixed solution of hydrochloric acid, bath raio is 1 ︰ 45, soaking time 40min.After immersion, extremely with 35 DEG C of warm water repeated flushing
It is neutral.
(4) cellulase treatment: under room temperature, it is 3g/L pectin that the reed straw that step (3) are handled, which is immersed in mass concentration,
In enzyme solutions, control pH value is 7, and temperature is 60 DEG C, soaking time 3h, and bath raio is 1 ︰ 45.After immersion, reed straw leaching
Bubble is in 2.5g/L laccase solution in mass concentration, and control pH value is 7.2, and temperature is 60 DEG C, soaking time 3h, and bath raio is 1 ︰
45.After immersion, with tap water repeated flushing to neutrality.
(5) organic solvent is handled: the reed straw that step (4) are handled being immersed in ethanol solution, temperature control is 50
DEG C, it is stirred continuously, mixing time 3h.After stirring, filtering removes filtrate, and remaining solid flocculent substance is cellulose
Fiber, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw cellulose in air.
(6) alkalization of reed straw pulp fibers element: by step (5), treated that reed straw cellulose is dissolved in 15g/L
NaOH solution, is added the auxiliary agent JL-EBZ of Accessories during Binzhou Ju Li Chemical Co., Ltd. production, and auxiliary agent JL-EBZ accounts for reed straw pulp
Mass values be 0.8%, dip time be 4.5 hours, 1 ︰ 6 of bath raio.
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into always
Forming apparatus, controlled at 15 DEG C, ageing time is 5.5 hours.
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2
Reaction, CS2Volume (mL) and reed straw pulp fibers element quality (g) than be 1 ︰ 140, the reaction time be 2 hours, react
Temperature is 70 DEG C.Cellulose sulfonate after yellow is reacted is added the NaOH solution that concentration is 80g/L and dissolves, cellulose sulfonic acid
The volume ratio of ester and NaOH solution is 1 ︰ 3.
(9) filtering and defoaming of viscose glue: by step (8) treated reed straw pulp fibers element sulphonic acid ester using filtering
Machine filtering；Filtered viscose glue is removed the bubble in reed straw pulp fibers element sulphonic acid ester using continuously and rapidly defoaming method
It removes, obtains viscose glue.
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 15
DEG C, the time is 7 hours, must reach the spinning solution of spinning Modal fibre, wherein the esterification degree of spinning solution is 69.8.
(11) the poly- limited public affairs of power chemical industry in Accessories during Binzhou the preparation before spinning: are added in step (10) treated spinning solution
The spin bath additive JL-FS of production is taken charge of, additional amount is the 0.19% of bath foam volume；Then the production of Changzhou letter AnDa Co., Ltd is added
Defoaming agent CD-FFA01, the additional amount of defoaming agent is the 0.05% of spinning solution volume；Wherein, the viscosity of spinning solution is
108.6Pa·s。
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath,
Coagulating bath by 75g/L H2SO4, 80g/L ZnSO4, 120g/L Na2SO4, remaining is water, and coagulation bath temperature is 40 DEG C, spinning
Speed is 40m/min, and Immersion time of the strand in coagulating bath is 1.5 seconds.
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand carries out spinneret drawing-off, this
Method is negative drawing-off, and degree of draft is -55.8%, and plasticizing drawing-off is 120%, and the drawing-off that bounces back after drawing-off is -3.5%.
(14) step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent solution (type that concentration is 0.6g/L
Number: the production of XS-K660A, Xu Shi Chemical Industry Science Co., Ltd), immersing the time is 0.8 hour, and solution temperature is room temperature, 1 ︰ of bath raio
18。
(15) desulfurization of fiber: step (14) treated fiber is immersed into the NaOH solution that concentration is 3.5g/L, is immersed
Time is 3 hours, and solution temperature is 80 DEG C, 1 ︰ 15 of bath raio.
(16) step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent solution (name that concentration is 0.1g/L
Claim: bleaching powder, the production of Guangzhou Yue Jia Chemical Industry Science Co., Ltd), immersing the time is 2 hours, and solution temperature is 40 DEG C, 1 ︰ of bath raio
12。
(17) washing of fiber: step (16) treated fiber being immersed in 85 DEG C of hot water, and the time is 1.5 hours,
1 ︰ 16 of bath raio.
(18) fiber oils: by the oil bath solution (model: DY- of step (17) treated fiber immerses 5g/L
NL1022, the production of Jining Hua Kai resin Co., Ltd), oil bath temperature is 75 DEG C, and the time is 2 hours, 1 ︰ 16 of bath raio.
(19) drying of fiber: by step (18), treated that fiber obtains Modal fibre c after drying and processing.
Embodiment 4
(1) clean: weighing 3000 grams of dry reed straw, reed straw is sawed it is broken, saw it is broken after every section length about 3~
4cm, by saw it is broken after reed straw cleaned with warm water, cleaning agent (all-round neutral cleaners, upper sea blue winged fining is added
The production of work Science and Technology Ltd.), cleaning agent dosage accounts for the 0.01% of reed straw, and reed straw quality (g) is water-soluble with cleaning agent
The bath raio of liquid product (mL) is 1 ︰ 100, and tap water repeated flushing is used after cleaning.
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 50, is added
The sodium hydroxide of 3g/L sodium metasilicate, 8g/L sodium sulfite and 6g/L, kiering temperature are 70 DEG C, and the kiering time is 110min.Kiering
After, with 35 DEG C of warm water repeated flushing to neutrality.
(3) pickling: under room temperature, it is 2g/L sulfuric acid and 2g/L that the reed straw that step (2) are handled, which is immersed in mass concentration,
In the mixed solution of hydrochloric acid, bath raio is 1 ︰ 40, soaking time 30.After immersion, with 30 DEG C of warm water repeated flushing into
Property.
(4) cellulase treatment: under room temperature, it is 2g/L pectin that the reed straw that step (3) are handled, which is immersed in mass concentration,
In enzyme solutions, control pH value is 6, and temperature is 55 DEG C, soaking time 2h, and bath raio is 1 ︰ 35.After immersion, reed straw leaching
Bubble is in 2g/L laccase solution in mass concentration, and control pH value is 6.5, and temperature is 55 DEG C, soaking time 3h, and bath raio is 1 ︰
40.After immersion, with tap water repeated flushing to neutrality.
(5) organic solvent is handled: the reed straw that step (4) are handled being immersed in ethanol solution, temperature control is 45
DEG C, it is stirred continuously, mixing time 2h.After stirring, filtering removes filtrate, and remaining solid flocculent substance is cellulose
Fiber, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw cellulose in air.
(6) alkalization of reed straw pulp fibers element: by step (5), treated that reed straw cellulose is dissolved in 10g/L
NaOH solution, is added the auxiliary agent JL-EBZ of Accessories during Binzhou Ju Li Chemical Co., Ltd. production, and auxiliary agent JL-EBZ accounts for reed straw pulp
Mass values be 0.4%, dip time be 4 hours, 1 ︰ 5 of bath raio.
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into always
Forming apparatus, controlled at 12 DEG C, ageing time is 5 hours.
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2
Reaction, CS2Volume (mL) and reed straw pulp fibers element quality (g) than be 1 ︰ 120, the reaction time be 1.5 hours, instead
Answering temperature is 60 DEG C.Cellulose sulfonate after yellow is reacted is added the NaOH solution that concentration is 50g/L and dissolves, cellulose sulphur
The volume ratio of acid esters and NaOH solution is 1 ︰ 2.
(9) filtering and defoaming of viscose glue: by step (8) treated reed straw pulp fibers element sulphonic acid ester using filtering
Machine filtering；Filtered viscose glue is removed the bubble in reed straw pulp fibers element sulphonic acid ester using continuously and rapidly defoaming method
It removes, obtains viscose glue.
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 8 DEG C,
Time is 5 hours, must reach the spinning solution of spinning Modal fibre, wherein the esterification degree of spinning solution is 67.9.
(11) the poly- limited public affairs of power chemical industry in Accessories during Binzhou the preparation before spinning: are added in step (10) treated spinning solution
The spin bath additive JL-FS of production is taken charge of, additional amount is the 0.15% of bath foam volume；Then the production of Changzhou letter AnDa Co., Ltd is added
Defoaming agent CD-FFA01, the additional amount of defoaming agent is the 0.02% of spinning solution volume；Wherein, the viscosity of spinning solution is
112.9Pa·s。
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath,
Coagulating bath by 70g/L H2SO4, 70g/L ZnSO4, 150g/L Na2SO4, remaining is water, and coagulation bath temperature is 50 DEG C, spinning
Speed is 35m/min, and Immersion time of the strand in coagulating bath is 1 second.
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand carries out spinneret drawing-off, this
Method is negative drawing-off, and degree of draft is -40%~-60%, and plasticizing drawing-off is 110%~135%, and the drawing-off that bounces back after drawing-off is -
1%~-4%.
(14) it is molten that step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent that concentration is 0.2~1.5g/L
Liquid (model: XS-K660A, Xu Shi Chemical Industry Science Co., Ltd production), immersing the time is 0.5~1 hour, and solution temperature is normal
Temperature, 1 ︰ 15~20 of bath raio.
(15) desulfurization of fiber: step (14) treated fiber is immersed into the NaOH solution that concentration is 3~4g/L, is immersed
Time is 2~4 hours, and solution temperature is 75~90 DEG C, 1 ︰ 10~20 of bath raio.
(16) it is molten that step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent that concentration is 0.1~0.5g/L
Liquid (title: bleaching powder, the production of Guangzhou Yue Jia Chemical Industry Science Co., Ltd), immersing the time is 1~3 hour, solution temperature 30
~50 DEG C, 1 ︰ 10~15 of bath raio.
(17) washing of fiber: step (16) treated fiber being immersed in 70~95 DEG C of hot water, and the time is 1~2
Hour, 1 ︰ 10~20 of bath raio.
(18) fiber oils: by the oil bath solution (model: DY- of step (17) treated fiber immerses 4~8g/L
NL1022, the production of Jining Hua Kai resin Co., Ltd), oil bath temperature is 75~85 DEG C, and the time is 1~4 hour, 1 ︰ 10 of bath raio~
20。
(19) drying of fiber: by step (18), treated that fiber obtains Modal fibre d after drying and processing.
Embodiment 5
(1) clean: weighing 3000 grams of dry reed straw, reed straw is sawed it is broken, saw it is broken after every section length about 4~
5cm, by saw it is broken after reed straw cleaned with warm water, cleaning agent (all-round neutral cleaners, upper sea blue winged fining is added
The production of work Science and Technology Ltd.), cleaning agent dosage accounts for the 0.05% of reed straw, and reed straw quality (g) is water-soluble with cleaning agent
The bath raio of liquid product (mL) is 1 ︰ 500, and tap water repeated flushing is used after cleaning.
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 60, is added
The sodium hydroxide of 6g/L sodium metasilicate, 8g/L sodium sulfite and 15g/L, kiering temperature are 80 DEG C, and the kiering time is 110min.Kiering
After, with 40 DEG C of warm water repeated flushing to neutrality.
(3) pickling: under room temperature, it is 4g/L sulfuric acid and 3g/L that the reed straw that step (2) are handled, which is immersed in mass concentration,
In the mixed solution of hydrochloric acid, bath raio is 1 ︰ 50, soaking time 50min.After immersion, extremely with 40 DEG C of warm water repeated flushing
It is neutral.
(4) cellulase treatment: under room temperature, it is 4g/L pectin that the reed straw that step (3) are handled, which is immersed in mass concentration,
In enzyme solutions, control pH value is 7.5, and temperature is 65 DEG C, soaking time 4h, and bath raio is 1 ︰ 55.After immersion, reed straw
Being immersed in mass concentration is in 3g/L laccase solution, and control pH value is 7, and temperature is 65 DEG C, soaking time 4h, and bath raio is 1 ︰
50.After immersion, with tap water repeated flushing to neutrality.
(5) organic solvent is handled: the reed straw that step (4) are handled being immersed in ethanol solution, temperature control is 60
DEG C, it is stirred continuously, mixing time 4h.After stirring, filtering removes filtrate, and remaining solid flocculent substance is cellulose
Fiber, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw cellulose in air.
(6) alkalization of reed straw pulp fibers element: by step (5), treated that reed straw cellulose is dissolved in 20g/L
NaOH solution, is added the auxiliary agent JL-EBZ of Accessories during Binzhou Ju Li Chemical Co., Ltd. production, and auxiliary agent JL-EBZ accounts for reed straw pulp
Mass values be 1.5%, dip time be 5 hours, 1 ︰ 8 of bath raio.
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into always
Forming apparatus, controlled at 18 DEG C, ageing time is 6 hours.
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2
Reaction, CS2Volume (mL) and reed straw pulp fibers element quality (g) than be 1 ︰ 150, the reaction time be 3 hours, react
Temperature is 80 DEG C.Cellulose sulfonate after yellow is reacted is added the NaOH solution that concentration is 100g/L and dissolves, cellulose sulphur
The volume ratio of acid esters and NaOH solution is 1 ︰ 4.
(9) filtering and defoaming of viscose glue: by step (8) treated reed straw pulp fibers element sulphonic acid ester using filtering
Machine filtering；Filtered viscose glue is removed the bubble in reed straw pulp fibers element sulphonic acid ester using continuously and rapidly defoaming method
It removes, obtains viscose glue.
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 20
DEG C, the time is 8 hours, must reach the spinning solution of spinning Modal fibre, wherein the esterification degree of spinning solution is 71.4.
(11) the poly- limited public affairs of power chemical industry in Accessories during Binzhou the preparation before spinning: are added in step (10) treated spinning solution
The spin bath additive JL-FS of production is taken charge of, additional amount is the 0.25% of bath foam volume；Then the production of Changzhou letter AnDa Co., Ltd is added
Defoaming agent CD-FFA01, the additional amount of defoaming agent is the 0.15% of spinning solution volume；Wherein, the viscosity of spinning solution is
117.6Pa·s。
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath,
Coagulating bath by 80g/L H2SO4, 90g/L ZnSO4, 150g/L Na2SO4, remaining is water, and coagulation bath temperature is 50 DEG C, spinning
Speed is 50m/min, and Immersion time of the strand in coagulating bath is 2 seconds.
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand carries out spinneret drawing-off, this
Method is negative drawing-off, and degree of draft is -56.8%, and plasticizing drawing-off is 125%, and the drawing-off that bounces back after drawing-off is -1.5%.
(14) step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent solution (type that concentration is 0.4g/L
Number: the production of XS-K660A, Xu Shi Chemical Industry Science Co., Ltd), immersing the time is 0.8 hour, and solution temperature is room temperature, 1 ︰ of bath raio
18。
(15) desulfurization of fiber: step (14) treated fiber is immersed into the NaOH solution that concentration is 3.5g/L, is immersed
Time is 2.5 hours, and solution temperature is 80 DEG C, 1 ︰ 15 of bath raio.
(16) step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent solution (name that concentration is 0.3g/L
Claim: bleaching powder, the production of Guangzhou Yue Jia Chemical Industry Science Co., Ltd), immersing the time is 1.5 hours, and solution temperature is 35 DEG C, bath raio
1 ︰ 12.
(17) washing of fiber: step (16) treated fiber being immersed in 85 DEG C of hot water, and the time is 1.5 hours,
1 ︰ 16 of bath raio.
(18) fiber oils: by the oil bath solution (model: DY- of step (17) treated fiber immerses 5g/L
NL1022, the production of Jining Hua Kai resin Co., Ltd), oil bath temperature is 82 DEG C, and the time is 3 hours, 1 ︰ 12 of bath raio.
(19) drying of fiber: by step (18), treated that fiber obtains Modal fibre e after drying and processing.
Performance evaluation example:
Strength property is carried out to Modal fibre a, b, c, d, e that specific embodiment 1~5 above-mentioned in the present invention is prepared
Test, test method with reference to GB/T-24218.3-2010 " textile, non-woven cloth test method third portion: ultimate strength and
The measurement of elongation at break ", the strength property of sample is measured using the full-automatic single fiber universl tester of FAVIMAT-BOBOT2,
Test sample is no less than 30, takes testing mean.Test result is as shown in table 1, wherein reed straw Modal fibre a, b,
C, d, e abbreviation fiber a, b, c, d, e, the Modal fibre of buying is from Shandong Zhong Xian textile technology Co., Ltd.
The mechanical property of table 1 reed straw Modal fibre a, b, c, d, e and the Modal fibre bought by oneself
As seen from Table 1, reed straw Modal fibre does breaking strength between 3.4~3.6cN/dtex, slightly below
The Modal fibre of buying, the dry elongation at break of reed straw Modal fibre are slightly above purchased between 12%~14%
Modal fibre；Reed straw Modal fibre wet breaking strength is slightly below purchased between 2.2~2.4cN/dtex
Modal fibre, the wet elongation at break of reed straw Modal fibre is between 12%~15%, not generation for slightly above purchasing
That fiber.On the whole, compared with the mechanical property of the Modal fibre of the mechanical property and buying of reed straw Modal fibre
It is close.Definition according to international chemical standard fibre office (BISFA) to Modal fibre, i.e., obtained high-strength by process
The regenerated cellulose of degree and high wet modulus, wet breaking strength is in 2.20cN/dtex or more, and wet elongation at break is less than 15%.
Reed straw Modal fibre prepared by the present invention substantially conforms to international chemical standard fibre office (BISFA) to Modal fibre
Definition, accordingly, it is believed that the present invention is a kind of Modal fibre by cellulose fibre prepared by raw material of reed straw.
Claims (10)
1. a kind of method for preparing Modal fibre as raw material using reed straw, it is characterised in that: the method includes walking as follows
It is rapid:
(1) clean: dry reed straw saw is broken, by saw it is broken after reed straw cleaned with warm water, cleaning agent is added,
Cleaning agent dosage accounts for the 0.01%~0.05% of reed straw, reed straw quality (g) and cleaning agent aqueous solution volume (mL)
Bath raio is 1 ︰ 100~500, and tap water repeated flushing is used after cleaning；
(2) soda boiling: under normal pressure, the reed straw of step (1) processing is subjected to kiering, wherein bath raio is 1 ︰ 40~60, is added suitable
Sodium metasilicate, sodium sulfite and the sodium hydroxide of concentration are measured, kiering temperature is 70 DEG C~80 DEG C, and the kiering time is 100~110min；
After kiering, with 35 DEG C~40 DEG C of warm water repeated flushing to neutrality；
(3) pickling: under room temperature, the mixing of sulfuric acid and hydrochloric acid that the reed straw that step (2) are handled is immersed in appropriate concentration is molten
In liquid, bath raio is 1 ︰ 40~50, and soaking time is 30~50min；After immersion, with 30 DEG C~40 DEG C of warm water repeated flushing
To neutrality；
(4) cellulase treatment: under room temperature, the reed straw that step (3) are handled being immersed in the pectinase solution of suitable concentration,
Controlling pH value is 6~7.5, and temperature is 55 DEG C~65 DEG C, and soaking time is 2~4h, and bath raio is 1 ︰ 35~55；After immersion,
Reed straw is immersed in the laccase solution of suitable concentration, and control pH value is 6.5~7.5, and temperature is 55 DEG C~65 DEG C, when immersion
Between be 3~4h, bath raio be 1 ︰ 40~50；After immersion, with tap water repeated flushing to neutrality；
(5) organic solvent handle: by step (4) handle reed straw be immersed in ethanol solution, temperature control for 45 DEG C~
It 60 DEG C, is stirred continuously, mixing time is 2~4h；After stirring, filtering removes filtrate, and remaining solid flocculent substance is fibre
Cellulose fiber, by solid flocculent substance tap water repeated flushing to neutrality, naturally dry can reed straw fiber in air
Element；
(6) alkalization of reed straw pulp fibers element: by step (5), treated that reed straw cellulose is dissolved in 10~20g/L
Auxiliary agent JL-EBZ is added in NaOH solution, and the mass values that auxiliary agent JL-EBZ accounts for reed straw pulp are 0.4~1.5%, when dipping
Between be 4~5 hours, 1 ︰ 5~8 of bath raio；
(7) reed straw pulp fibers element is experienced: by step (6), treated that reed straw pulp fibers element is put into experienced set
Standby, controlled at 12~18 DEG C, ageing time is 5~6 hours；
(8) yellow of reed straw pulp fibers element: by step (7) treated reed straw pulp fibers element and CS2Reaction,
Reaction time is 1.5~3 hours, and reaction temperature is 60~80 DEG C；Concentration is added in cellulose sulfonate after yellow is reacted
The NaOH solution of 50~100g/L dissolves, and the volume ratio of cellulose sulfonate and NaOH solution is 1 ︰ 2~4；
(9) step (8) treated reed straw pulp fibers element sulphonic acid ester the filtering and defoaming of viscose glue: is used into filter mistake
Filter；By filtered viscose glue using continuously and rapidly defoaming method by the bubble removal in reed straw pulp fibers element sulphonic acid ester,
Obtain viscose glue；
(10) maturation of spinning solution: by step (9) treated viscose glue maturation in maturation bucket, controlled at 8~20 DEG C,
Time is 5~8 hours, must reach the spinning solution of spinning Modal fibre；
(11) spin bath additive JL-FS the preparation before spinning: is added in step (10) treated spinning solution；Then plus
Enter defoaming agent CD-FFA01, the additional amount of defoaming agent is the 0.02~0.15% of spinning solution volume；Wherein, the viscosity of spinning solution
For 100~120Pas；
(12) it comes into being the preparation of strand: by step (11) treated spinning solution solidification forming in spinning coagulation bath, solidification
Bath is by H2SO4、ZnSO4、Na2SO4It is formed with water, coagulation bath temperature is 35~50 DEG C, and spinning speed is 35~50m/min, strand
Immersion time in coagulating bath is 0.8~2 second；
(13) come into being the drawing-off and post-processing of strand: to step (12), treated that nascent strand sprays under suitable degree of draft
Filament drafting, the method are negative drawing-off, and plasticizing drawing-off is 110%~135%, and the drawing-off that bounces back after drawing-off is -1%~-4%；
(14) step (13) treated fiber the defoaming of fiber: is immersed into the defoaming agent solution that concentration is 0.2~1.5g/L, leaching
The angle of incidence is 0.5~1 hour, and solution temperature is room temperature, 1 ︰ 15~20 of bath raio；
(15) desulfurization of fiber: step (14) treated fiber is immersed into the NaOH solution that concentration is 3~4g/L, immerses the time
It is 2~4 hours, solution temperature is 75~90 DEG C, 1 ︰ 10~20 of bath raio；
(16) step (15) treated fiber the bleaching of fiber: is immersed into the bleaching agent solution that concentration is 0.1~0.5g/L, leaching
The angle of incidence is 1~3 hour, and solution temperature is 30~50 DEG C, 1 ︰ 10~15 of bath raio；
(17) washing of fiber: step (16) treated fiber being immersed in 70~95 DEG C of hot water, and the time is 1~2 hour,
1 ︰ 10~20 of bath raio；
(18) fiber oils: by the oil bath solution of step (17) treated fiber immerses 4~8g/L, oil bath temperature is 75~
85 DEG C, the time is 1~4 hour, 1 ︰ 10~20 of bath raio；
(19) drying of fiber: by step (18), treated, and fiber obtains Modal fibre after drying and processing.
2. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
Every section length about 2~5cm after reed straw saw is broken in the step (1).
3. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
Sodium silicate silicate is 3~6g/L in the step (2), concentration of sodium sulfite is 3~8g/L and naoh concentration be 6~
15g/L。
4. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
Sulfuric acid concentration is 2~4g/L in the step (3) and concentration of hydrochloric acid is 2~3g/L.
5. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
Pectin enzyme concentration is 2~4g/L in the step (4), and laccase concentration is 2~3g/L.
6. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
CS in the step (8)2Volume (mL) and reed straw pulp fibers element quality (g) than for 1 ︰ 120~150.
7. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
The esterification degree of spinning solution is 65~75 in the step (10).
8. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
The additional amount of spin bath additive JL-FS is the 0.15~0.25% of bath foam volume in the step (11).
9. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, it is characterised in that:
H in the step (12)2SO4Concentration be 70~80g/L, ZnSO4Concentration be 70~90g/L, Na2SO4Concentration be 80
~150g/L.
10. a kind of method for preparing Modal fibre as raw material using reed straw according to claim 1, feature exist
In: degree of draft is -40%~-60% in the step (13).
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| CN110791878A (en) * | 2019-11-06 | 2020-02-14 | 江南大学 | Preparation method of high-adsorbability artificial fiber membrane |
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