CN108893796A - A kind of plant source modified cellulose fibre - Google Patents
A kind of plant source modified cellulose fibre Download PDFInfo
- Publication number
- CN108893796A CN108893796A CN201810699421.6A CN201810699421A CN108893796A CN 108893796 A CN108893796 A CN 108893796A CN 201810699421 A CN201810699421 A CN 201810699421A CN 108893796 A CN108893796 A CN 108893796A
- Authority
- CN
- China
- Prior art keywords
- pulp
- cellulose fibre
- plant
- spinning
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- 239000000835 fiber Substances 0.000 claims abstract description 45
- 238000002360 preparation method Methods 0.000 claims abstract description 43
- 229920002678 cellulose Polymers 0.000 claims abstract description 33
- 239000001913 cellulose Substances 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 230000008961 swelling Effects 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- 239000002956 ash Substances 0.000 claims abstract description 11
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- 239000000428 dust Substances 0.000 claims abstract description 6
- 238000002203 pretreatment Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 58
- 238000009987 spinning Methods 0.000 claims description 57
- 239000002608 ionic liquid Substances 0.000 claims description 51
- 238000000034 method Methods 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 36
- 239000000284 extract Substances 0.000 claims description 32
- 239000002245 particle Substances 0.000 claims description 32
- 239000007864 aqueous solution Substances 0.000 claims description 30
- DAEPDZWVDSPTHF-UHFFFAOYSA-M sodium pyruvate Chemical compound [Na+].CC(=O)C([O-])=O DAEPDZWVDSPTHF-UHFFFAOYSA-M 0.000 claims description 30
- 238000009960 carding Methods 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 23
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 claims description 20
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 20
- 239000003381 stabilizer Substances 0.000 claims description 20
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- 238000012805 post-processing Methods 0.000 claims description 16
- 238000004090 dissolution Methods 0.000 claims description 15
- 108010002430 hemicellulase Proteins 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- 229940054269 sodium pyruvate Drugs 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 14
- 238000010792 warming Methods 0.000 claims description 14
- 229920002101 Chitin Polymers 0.000 claims description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 13
- 230000000694 effects Effects 0.000 claims description 13
- 229940059442 hemicellulase Drugs 0.000 claims description 13
- 239000008187 granular material Substances 0.000 claims description 11
- 108090000790 Enzymes Proteins 0.000 claims description 10
- 102000004190 Enzymes Human genes 0.000 claims description 10
- 229940088598 enzyme Drugs 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 10
- 230000008020 evaporation Effects 0.000 claims description 10
- AVXURJPOCDRRFD-UHFFFAOYSA-N hydroxylamine group Chemical group NO AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 10
- 239000000473 propyl gallate Substances 0.000 claims description 10
- 229940075579 propyl gallate Drugs 0.000 claims description 10
- 235000010388 propyl gallate Nutrition 0.000 claims description 10
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 4
- 125000002252 acyl group Chemical group 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims 1
- 239000004753 textile Substances 0.000 abstract description 2
- 239000004744 fabric Substances 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 62
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 25
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 16
- 241000209094 Oryza Species 0.000 description 10
- 235000007164 Oryza sativa Nutrition 0.000 description 10
- 235000009566 rice Nutrition 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000007664 blowing Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 229920000742 Cotton Polymers 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- UHOPWFKONJYLCF-UHFFFAOYSA-N 2-(2-sulfanylethyl)isoindole-1,3-dione Chemical compound C1=CC=C2C(=O)N(CCS)C(=O)C2=C1 UHOPWFKONJYLCF-UHFFFAOYSA-N 0.000 description 4
- 241001145025 Saussurea involucrata Species 0.000 description 4
- 241001593750 Turcica Species 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 4
- 238000004061 bleaching Methods 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000012476 oxidizable substance Substances 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241000195493 Cryptophyta Species 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 244000082204 Phyllostachys viridis Species 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000419 plant extract Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 2
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000006196 deacetylation Effects 0.000 description 2
- 238000003381 deacetylation reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000007380 fibre production Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000004627 regenerated cellulose Substances 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 229920000875 Dissolving pulp Polymers 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001449 anionic compounds Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 235000020710 ginseng extract Nutrition 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 150000002891 organic anions Chemical class 0.000 description 1
- 150000002892 organic cations Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229940107700 pyruvic acid Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000005418 vegetable material Substances 0.000 description 1
- 239000002699 waste material Substances 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
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention provides a kind of plant source modified cellulose fibre, belongs to textile fabric field, and preparation method includes:Swelling, pre-treatment step;The swelling step:Fiber pulp is immersed in deionized water, swelling is thoroughly mixed;Content of cellulose >=96.5% of the pulp, content of ashes≤0.06, small dust≤50mm2/ kg, dynamic viscosity 16.15-18.25mPa.s, 800 or less content of the degree of polymerization is less than 6%.The pre-treatment step:Pulp after swelling is dehydrated within 20%, is then immersed pulp in pretreating agent, impregnating by pressure pretreatment, pretreatment time 30-50mn;The dosage of the pretreating agent is 3-10 times of pulp quality.Functionality solvents prepared by the present invention spin cellulose fibre, and doing breaking strength is 3.83-3.92 cN/dtex;Wet breaking strength is 3.31-3.68 cN/dtex.
Description
Technical field
The present invention relates to a kind of cellulose fibre and preparation method thereof, especially a kind of plant source modified cellulose fibre,
Belong to field of textiles.
Background technique
Solvent-spun cellulose fibre refers to by obtained cellulose is extracted and purified from the vegetable materials such as cotton linter, timber
For raw material, through being solvent with N monomethyl beautiful jade, fiber made from spinning after directly dissolving.It is fine that comparison routine techniques produces regeneration
The industrial pollution of cellulose fiber, production process is fewer, and fibre property has hygroscopicity possessed by regenerated celulose fibre
Good, comfortable and easy to wear outer, the relative wet strength and wet modulus of fiber are high.The product of dry production diversified forms can be used, but to being before the moon
Only, throw labor market is still only staple fiber.
Ionic liquid is completely by organic cation and organic/inorganic anion group as a kind of novel " green solvent "
At, in room temperature or be bordering on the organic salt being in a liquid state at room temperature, with the characteristic that conventional organic solvents are incomparable, such as vapour pressure
It is extremely low, fusing point is low, very strong solvability, preferable thermal stability, wider liquid journey range, structure can design, recyclable makes
With etc., good application prospect has been shown in chemical fields such as separating and extracting, catalysis, materials synthesis, electrochemistry.In recent years
Come, the great attention of academia and business circles is caused with the new process that ionic liquid prepares material of regenerated cellulose.It has sent out
Existing several ionic liquid is known as good dissolubility to fiber, and can be used to prepare regenerated celulose fibre and regeneration
Cellulose membrane.In the production of material of regenerated cellulose, cellulose solution preparation is a crucial technology.It is fine only in solution
It ties up the plain degree of polymerization to meet the requirements, and is dissolved thoroughly, uniformly in ionic liquid, it is preferable could steadily to prepare spinning properties
Product.If be not thorough after dissolution, production technology is just unstable, be easy to cause broken end, and fiber spinnability is bad.
At present, it has been reported that the method for preparing cellulose/ionic liquid solution generally use dissolution kettle, be exactly solvent
Ionic liquid and cellulose are added to the container in batch, are then heated while stirring, until forming homogeneous solution.Patent
Dissolution process in CN1491974A just belongs to this method.The shortcomings that this method is that dissolution time is long, low efficiency.Although rising
High solution temperature can be accelerated to dissolve, but often result in cellulose excessive degradation, cause fiber strength decline obvious.
China Patent No. is CN200710118242.0, discloses one kind and continuously prepares cellulose/ionic liquid solution
Cellulose and ionic liquid are mainly first mixed into ooze shape mixture by method, then again add the ooze shape mixture
Enter the spout of screw extruder, continuous-dissolution obtains cellulose/ionic liquid solution in the outlet of screw extruder.Fiber
The mixture of ooze shape is formed after element and ionic liquid mixing, the mixture of the ooze shape does not contain dissociated ion liquid, has
Do not flow automatically, non-settling characteristic.The present invention processes the mixture of the ooze shape using screw extruder, utilizes cutting for extruder
The effect of cutting can be improved the dissolved efficiency of cellulose, shorten dissolution time, and cellulose is avoided seriously to degrade.This method is main
It is quickly to be dissolved using screw extruder to cellulose, the process in such method due to screw extruder is shorter, shearing
Ability is lower, therefore ionic liquid is made to be difficult in a short time to be completely dissolved cellulose, causes the fiber strand silk of preparation
Phenomena such as broken end.
In patent WO2006/000197A1, cellulose first is dispersed in water, then add in ionic liquid into
Row dissolution.It is well known that water is known as very strong swelling action to fiber, therefore the technology has certain side to cellulose dissolution
It helps.But because the ability that the water remained in pulp can make ionic liquid lose dissolution cellulose, causes ionic liquid
Dosage is excessive, and ionic liquid is caused to waste and recycle difficulty.
Meanwhile in the prior art, do not find that plant extracts is added to solvent to be spun in fiber, has function with preparation also
The report of the solvent-spun cellulose fibre of energy property, misses to adapt to the demand of fibre in differentiation.
Summary of the invention
For the appearance of the prior art solvent-spun cellulose fibre functionality is poor, strength low, fiber strand silk broken end is existing
As, the biggish technological deficiency of ionic liquid dosage, the present invention provides a kind of plant source modified cellulose fibre to reach above-mentioned
Goal of the invention, technical solution provided by the invention are:
1, it is swollen:Fiber pulp is immersed in deionized water, swelling is thoroughly mixed;The pulp is Cotton Pulp, wood pulp
The one or more of the dregs of rice, hemp dissolving pulp, bamboo pulp, preferably Cotton Pulp;Content of cellulose >=96.5% of the pulp, ash content contain
Amount(575℃)≤ 0.06, small dust≤50mm2/ kg, dynamic viscosity 16.15-18.25mPa.s, 800 or less content of the degree of polymerization are small
In 6%;
It is swollen using deionized water, the content of ash content in pulp can be reduced to greatest extent, improve the quality of finished product;Institute
Stating 25 DEG C of conductivity of deionized water is≤0.8us/cm;Oxidizable substance content≤0.05mg/L;Absorbance(254nm, 1cm light
Journey)≤0.01;Evaporation residue(105±2℃)≤1mg/L.Preparing cellulose fibre using solvent spinning method is a fining
Work technology, it is quite unmature yet so far, therefore have strict requirements to water quality, the quality of pulp, because being directly related to subsequent
The quality of product and the detection of product index, therefore we are using above-mentioned indices are stringent, the higher deionized water of accuracy
And pulp;
It is described to be stirred the time as 30-50min;The deionized water temperature is 40-50 DEG C;It is described to be stirred swelling time
For 20-30min;
2, it pre-processes:By step(1)Pulp after swelling is dehydrated within 20%, is immersed in pretreating agent pulp after dehydration, is added
Press pretreatment, pretreatment time 30-50mn;The dosage of the pretreating agent is 3-10 times of pulp quality;
The preparation method of the pretreating agent:
The ionic liquid solution that concentration is 3-10% is warming up to 30-50 DEG C of temperature, pulp quality score 0.5-2% isomery ten is added
Triol stirs 5-10min, and carding agent is added, is again stirring for 5-10min, by being ultrasonically treated twice, obtains pretreating agent;It is described
First time ultrasonic time 15-20min, supersonic frequency 150-180KHz;Second of ultrasonic time is 45-60min, secondary
Supersonic frequency is 100-120 KHz.
The additional amount of the carding agent is the 10-30% of the pretreating agent quality;
The carding agent includes according to parts by weight following component, 1-2 parts of sodium bicarbonates, 0.2-0.5 parts of plant functions extractions
Composition granule, 3-10 parts of dehydrated alcohols, 0.05-0.1 portions of hemicellulases, 1.5-5 parts of chitin, 20-50 parts of 40-50% concentration
Ionic liquid aqueous solution;
Further, the preparation method of the carding agent:
(1)The ionic liquid aqueous solution for configuring 40-50% concentration, is warming up to 70-80 DEG C for ionic liquid aqueous solution, then by first
Shell element is even added in ionic liquid aqueous solution, stirring and dissolving, mixing speed 500-600r/min, stirring and dissolving time 5-
Chitin-ionic liquid aqueous solution is made in 10min;
(2)Plant function extract particles are mixed to 50-70 DEG C of stirring and dissolving of heating, stirring and dissolving time 30- with dehydrated alcohol
Plant granule annex solution is made in 40min;
(3)By step(1)Chitin-the ionic liquid aqueous solution and step of preparation(2)The plant granule annex solution of preparation mixes,
50 DEG C are cooled to solution to stir evenly hereinafter, hemicellulase and sodium bicarbonate is added, and carding agent is made;
The chitin, deacetylation >=96.5%, viscosity 550-700mPa.s, ignition residue≤0.6%;
The hemicellulase, enzyme activity storage rate >=88.5%, enzyme activity are ten thousand U/g of 95-100, effective component content >=99.5%.
3, dissolution evaporation:Pretreated pulp is de- dry, it is ground into pulp particle, stabilizer, galla turcica is then added
Propyl propionate, NMMO solvent mix rising temperature for dissolving into cellulose solution;Cellulose solution is entered into cold boiler and carries out vacuum steaming
Hair forms spinning solution;
The additional amount of the stabilizer is the 2-4.5% for taking off dry pulp quality;The stabilizer is azanol, tetrahydrofuran, pyruvic acid
The mixture of sodium;In the stabilizer, azanol, tetrahydrofuran, Sodium Pyruvate mass ratio be 5-10:20-40:2-3;Preferably
5:20:3;
The additional amount of the propylgallate is the 0.5-1.5% for taking off dry pulp quality;
The mass fraction of over dry pulp is 70-80% after the de- dry pulp dregs of rice(Over dry pulp accounts for the quality of de- dry rear pulp gross mass
Percentage);The not super more 8mm of partial size longest of the smashed pulp particle;
The concentration of the NMMO solvent is 65-70%;
The mass ratio of the de- dry pulp dregs of rice and NMMO solvent is 2:5-7;
The warming temperature is 80-90 DEG C;
The reduction vaporization temperature is 108-115 DEG C, vacuum degree 13.2-14.6kpa.
4, spinning and post-processing:Manufactured spinning solution is entered filter to be filtered, removes impurity;Impurity is transferred to
Rinsing bowl carries out washing recovery section NMMO solvent, while filtered spinning solution and the plant function precursor liquid of preparation being pressed
According to 10:Enter spinning pump after the mass ratio mixing of 0.5-1, is then spun by spinning, the obtained functionality solvents of post-processing fine
Cellulose fiber.
The component of the plant function precursor liquid includes:
Filtered spinning solution 17-19 parts, 0.05-0.15 parts of propylgallate, 8-10 parts of plant function extract particles,
0.1-0.3 parts of mixed aid;The mixed aid is:Glycerol, dimethyl sulfoxide, Sodium Pyruvate mixture;The mixing helps
Glycerol in agent, dimethyl sulfoxide, Sodium Pyruvate mass ratio be 5-8:1-2:0.5-1;
The plant function extract particles are:Herba Pileae Scriptae extract, Saussurea involucrata extract, marine algae extract, ginseng extract, Ma
The one or more of card extract;It is commercially available;The plant function extract particles fineness 150-200 mesh, content of ashes≤
0.5%, moisture content≤1%, total plate count < 500cfu/g, content of beary metal≤0.1ppm;
In the spinning process, spinning speed 65-80m/min, air blowing temperature is 15-18 DEG C, air mass flow 50-
60L/H, blowing relative humidity are 35-45%;Spinning air gap 65-100mm;
The postprocessing working procedures include washing, oiling, drying, and remove bleaching process, further retain fiber strength, keep fiber
Original appearance.
50 ± 3 DEG C of the washing temperature;The finish that oils is Daikin production(DAIKIN), model TG-580S,
Finish is 15-25g/L, pH value 3-5 using concentration;
The drying temperature is 110-130 DEG C.
Plant source modified cellulose fibre strength prepared by the present invention is high, has preferable wet modulus and elongation at break,
Fiber production process process stabilizing, in fiber end processing sequences, it is not easy to generate breakage phenomena, good spinnability;Meanwhile in life
For different plant extract particles are added during producing, the solvent-spun cellulose fibre of preparation shows different functionality
Feature.
By adopting the above-described technical solution, having the technical effect that of reaching of the present invention:
1, plant source modified cellulose fibre strength prepared by the present invention is high, and doing breaking strength is 3.83-3.92 cN/dtex;
Wet breaking strength is 3.31-3.68 cN/dtex.
2, plant source modified cellulose fibre prepared by the present invention, dry state modulus are 35.7-37.2;Hygrometric state modulus is
33.2-35.9;Illustrate that functionality solvents prepared by the present invention spin cellulose fibre and have good physical mechanical property and form
Stability.
3, plant source modified cellulose fibre prepared by the present invention, density are 1.46-1.47 g.cm-3 ;Water Peng's humidity is
52-55%;Yarn washing shrinkage is 0.5-0.7%;Colluding with breaking strength is 2.08-2.25 cN/dtex.
4, plant source modified cellulose fibre process stabilizing prepared by the present invention, in fiber end processing sequences, it is not easy to
Generate breakage phenomena, good spinnability.
5, the present invention can make the fiber of preparation due to that can add different plant extracts completely in process of production
Different functional characteristics is presented.
Specific embodiment
A kind of preparation method of the plant source modified cellulose fibre of embodiment 1, includes the following steps:
1, it is swollen:Fiber pulp is immersed in deionized water, swelling is thoroughly mixed;Pulp is Cotton Pulp;The fibre of pulp
Tie up cellulose content 97.5%, content of ashes(575℃)0.05, small dust 35mm2/ kg, dynamic viscosity 16.15mPa.s, the degree of polymerization 800
Following content is less than 6%;25 DEG C of conductivity of deionized water are 0.7us/cm;Oxidizable substance content 0.05mg/L;Absorbance
(254nm, 1cm light path)0.01;Evaporation residue(105±2℃)0.8mg/L;Being stirred the time is 30min;Deionization water temperature
Degree is 40 DEG C;Being stirred swelling time is 20min;
2, it pre-processes:By step(1)Pulp after swelling is dehydrated to 18%, is immersed to pressurize in pretreating agent by pulp after dehydration and be soaked
Stain pretreatment, pretreatment time 30mn;The dosage of pretreating agent is 4 times of pulp quality;
The preparation method of pretreating agent:
The ionic liquid solution that concentration is 3% is warming up to temperature 50 C, 0.5% isomerous tridecanol of pulp quality score is added, stirs
5min is mixed, carding agent is added, is again stirring for 5min, by being ultrasonically treated twice, obtains pretreating agent;First time ultrasonic time
15min, supersonic frequency 150KHz;Second of ultrasonic time is 45min, and twice ultrasonic frequency is 120 KHz;Carding agent adds
Enter 10% that amount is the pretreating agent quality;
Carding agent, according to parts by weight, include following component, 1 part of sodium bicarbonate, 0.3 part of plant function extract particles, 3 parts
Dehydrated alcohol, 0.05 portion of hemicellulase, 1.8 parts of chitin, 20 parts of the ionic liquid aqueous solution of 40-50% concentration;
The preparation method of carding agent:
(1)The ionic liquid aqueous solution for configuring 40-50% concentration, is warming up to 70 DEG C for ionic liquid aqueous solution, then by chitin
It is even added in ionic liquid aqueous solution, stirring and dissolving, mixing speed 500r/min, first is made in stirring and dissolving time 5min
Shell element-ionic liquid aqueous solution;
(2)Plant function extract particles mix with dehydrated alcohol to 50 DEG C of stirring and dissolvings of heating, stirring and dissolving time 30min,
Plant granule annex solution is made;
(3)By step(1)Chitin-the ionic liquid aqueous solution and step of preparation(2)The plant granule annex solution of preparation mixes,
50 DEG C are cooled to solution to stir evenly hereinafter, hemicellulase and sodium bicarbonate is added, and carding agent is made;Chitin takes off second
Acyl degree 96.5%, viscosity 550mPa.s, ignition residue 0.6%;Hemicellulase, enzyme activity storage rate 88.5%, enzyme activity are 950,000 U/
G, effective component content 99.5%.
3, dissolution evaporation:Pretreated pulp is de- dry, it is ground into pulp particle, stabilizer, galla turcica is then added
Propyl propionate, NMMO solvent mix rising temperature for dissolving into cellulose solution;Cellulose solution is entered into cold boiler and carries out vacuum steaming
Hair forms spinning solution;
The additional amount of stabilizer is the 2-4.5% for taking off dry pulp quality;Stabilizer is the mixing of azanol, tetrahydrofuran, Sodium Pyruvate
Object;In stabilizer, azanol, tetrahydrofuran, Sodium Pyruvate mass ratio be 5:2:2-3;The additional amount of propylgallate is de-
The 1.5% of dry pulp quality;
The mass fraction of over dry pulp is 70% after the de- dry pulp dregs of rice(Over dry pulp accounts for the quality percentage of de- dry rear pulp gross mass
Than);
The not super more 8mm of the partial size longest of smashed pulp particle;The concentration of NMMO solvent is 65%;The de- dry pulp dregs of rice and NMMO are molten
The mass ratio of agent is 2:5;Warming temperature is 80 DEG C;It is 108 DEG C that temperature, which is evaporated under reduced pressure, vacuum degree 13.2kpa.
4, spinning and post-processing:Manufactured spinning solution is entered filter to be filtered, removes impurity;Impurity is transferred to
Rinsing bowl carries out washing recovery section NMMO solvent, while filtered spinning solution and the plant function precursor liquid of preparation being pressed
According to 10:Enter spinning pump after 0.5 mass ratio mixing, functionality solvents then are made by spinning, post-processing and spin fiber
Cellulose fiber.
The component of plant function precursor liquid includes:
17 parts of filtered spinning solution, 0.05 part of propylgallate, 8 parts of plant function extract particles, mixed aid 0.1
Part;Mixed aid is:Glycerol, dimethyl sulfoxide, Sodium Pyruvate mixture;Glycerol, dimethyl sulfoxide, acetone in mixed aid
The mass ratio of sour sodium is 5:1:0.5;
Plant function extract particles are:Herba Pileae Scriptae extract, it is commercially available;Plant function extract particles fineness 150-180 mesh, ash
Divide content 0.5%, moisture content 1%, total plate count < 500cfu/g, content of beary metal≤0.1ppm;
In spinning process, spinning speed 65m/min, air blowing temperature is 15 DEG C, air mass flow 50L/H, and blowing is opposite
Humidity is 35%;Spinning air gap 650mm;
Postprocessing working procedures include washing, oiling, drying, and remove bleaching process, further retain fiber strength, keep fiber original
Appearance.
50 DEG C of washing temperature;The finish that oils is Daikin production(DAIKIN), model TG-580S, finish uses dense
Degree is 15g/L, pH value 3;
Drying temperature is 110 DEG C.
A kind of preparation method of the plant source modified cellulose fibre of embodiment 2, includes the following steps:
1, it is swollen:Fiber pulp is immersed in deionized water, swelling is thoroughly mixed;Pulp is Cotton Pulp;The fibre of pulp
Tie up cellulose content 96.5%, content of ashes(575℃)0.06, small dust 50mm2/ kg, dynamic viscosity 18.25mPa.s, the degree of polymerization 800
Following content is less than 6%;
25 DEG C of conductivity of deionized water are 0.8us/cm;Oxidizable substance content 0.05mg/L;Absorbance(254nm, 1cm light path)
0.01;Evaporation residue(105±2℃)0.8mg/L;
Being stirred the time is 45min;Deionized water temperature is 45 DEG C;Being stirred swelling time is 25min;
2, it pre-processes:By step(1)Pulp after swelling is dehydrated to 16%, is immersed pulp in pretreating agent after dehydration, pressurization leaching
Stain pretreatment, pretreatment time 45mn;The dosage of pretreating agent is 6 times of pulp quality;
The preparation method of pretreating agent:
The ionic liquid solution that concentration is 5% is warming up to 46 DEG C of temperature, 1.5% isomerous tridecanol of pulp quality score is added, stirs
5-10min is added carding agent, is again stirring for 5min, by being ultrasonically treated twice, obtains pretreating agent;First time ultrasonic time
15min, supersonic frequency 180KHz;Second of ultrasonic time is 60min, and twice ultrasonic frequency is 100 KHz.
The additional amount of carding agent is the 15% of the pretreating agent quality;
Carding agent, according to parts by weight, include following component, 1.5 parts of sodium bicarbonates, 0.3 part of plant function extract particles, 5
Part dehydrated alcohol, 0.1 portion of hemicellulase, 1.5 parts of chitin, 30 parts of the ionic liquid aqueous solution of 40-50% concentration;
The preparation method of carding agent:
(1)Ionic liquid aqueous solution is warming up to 70 DEG C by the ionic liquid aqueous solution for configuring 45% concentration, then that chitin is equal
Even to be added in ionic liquid aqueous solution, crust is made in stirring and dissolving, mixing speed 500r/min, stirring and dissolving time 7min
Element-ionic liquid aqueous solution;
(2)Plant function extract particles mix with dehydrated alcohol to 55 DEG C of stirring and dissolvings of heating, stirring and dissolving time 35min,
Plant granule annex solution is made;
(3)By step(1)Chitin-the ionic liquid aqueous solution and step of preparation(2)The plant granule annex solution of preparation mixes,
50 DEG C are cooled to solution to stir evenly hereinafter, hemicellulase and sodium bicarbonate is added, and carding agent is made;
Chitin, deacetylation 96.5%, viscosity 600mPa.s, ignition residue 0.4%;
Hemicellulase, enzyme activity storage rate 88.5%, enzyme activity are 1,000,000 U/g, effective component content 99.5%.
3, dissolution evaporation:Pretreated pulp is de- dry, it is ground into pulp particle, stabilizer, galla turcica is then added
Propyl propionate, NMMO solvent mix rising temperature for dissolving into cellulose solution;Cellulose solution is entered into cold boiler and carries out vacuum steaming
Hair forms spinning solution;
The additional amount of stabilizer is take off dry pulp quality 3%;Stabilizer is the mixture of azanol, tetrahydrofuran, Sodium Pyruvate;
In stabilizer, azanol, tetrahydrofuran, Sodium Pyruvate mass ratio be 5:20:3;The additional amount of propylgallate is de- dry pulp
The 1.0% of dregs of rice quality;
The mass fraction of over dry pulp is 75% after the de- dry pulp dregs of rice(Over dry pulp accounts for the quality percentage of de- dry rear pulp gross mass
Than);The not super more 8mm of partial size longest of the smashed pulp particle;
The concentration of NMMO solvent is 65%;
The mass ratio of the de- dry pulp dregs of rice and NMMO solvent is 2:5;
Warming temperature is 85 DEG C;
It is 110 DEG C that temperature, which is evaporated under reduced pressure, vacuum degree 13.5kpa.
4, spinning and post-processing:Manufactured spinning solution is entered filter to be filtered, removes impurity;Impurity is transferred to
Rinsing bowl carries out washing recovery section NMMO solvent, while filtered spinning solution and the plant function precursor liquid of preparation being pressed
According to 10:Enter spinning pump after 1 mass ratio mixing, functionality solvents then are made by spinning, post-processing and spin cellulose
Fiber.
The component of plant function precursor liquid includes:
18 parts of filtered spinning solution, 0.1 part of propylgallate, 9 parts of plant function extract particles, mixed aid 0.2
Part;Mixed aid is:Glycerol, dimethyl sulfoxide, Sodium Pyruvate mixture;Glycerol, dimethyl sulfoxide, acetone in mixed aid
The mass ratio of sour sodium is 6:1:1;
Plant function extract particles are:The mixture of Saussurea involucrata extract, marine algae extract is commercially available;Wherein saussurea involucrata is extracted
Object, marine algae extract mass ratio be 3:2;200 mesh of plant function extract particles fineness, content of ashes 0.5%, moisture content
1%, total plate count 500cfu/g, content of beary metal 0.05ppm;
In spinning process, spinning speed 70m/min, air blowing temperature is 16 DEG C, air mass flow 55L/H, and blowing is opposite
Humidity is 45%;Spinning air gap 65mm;
Postprocessing working procedures include washing, oiling, drying, and remove bleaching process, further retain fiber strength, keep fiber original
Appearance.
52 DEG C of washing temperature;The finish that oils is Daikin production(DAIKIN), model TG-580S, finish uses dense
Degree is 20g/L, pH value 5;
Drying temperature is 120 DEG C.
A kind of preparation method of the plant source modified cellulose fibre of embodiment 3, includes the following steps:
1, it is swollen:Fiber pulp is immersed in deionized water, swelling is thoroughly mixed;Pulp is Cotton Pulp, bamboo pulp
Mix pulp, wherein Cotton Pulp, bamboo pulp mass ratio be 2:1;The content of cellulose 96.5% of pulp, content of ashes(575℃)
0.06, small dust 45mm2/ kg, dynamic viscosity 17.25mPa.s, 800 or less content of the degree of polymerization is less than 6%;
25 DEG C of conductivity of deionized water are 0.6us/cm;Oxidizable substance content 0.05mg/L;Absorbance(254nm, 1cm light path)
0.01;Evaporation residue(105±2℃)0.5mg/L;
Being stirred the time is 50min;Deionized water temperature is 50 DEG C;Being stirred swelling time is 25min;
2, it pre-processes:By step(1)Pulp after swelling is dehydrated to 16%, is immersed pulp in pretreating agent after dehydration, pressurization leaching
Stain pretreatment, pretreatment time 45mn;The dosage of pretreating agent is -10 times of pulp quality;
The preparation method of pretreating agent:
The ionic liquid solution that concentration is 10% is warming up to temperature 50 C, 1.8% isomerous tridecanol of pulp quality score is added, stirs
8min is mixed, carding agent is added, is again stirring for 8min, by being ultrasonically treated twice, obtains pretreating agent;First time ultrasonic time
20min, supersonic frequency 150KHz;Second of ultrasonic time is 60min, and twice ultrasonic frequency is 100 KHz.
The additional amount of carding agent is the 30% of the pretreating agent quality;
Carding agent, according to parts by weight, include following component, 1 part of sodium bicarbonate, 0.5 part of plant function extract particles, 10
Part dehydrated alcohol, 0.1 portion of hemicellulase, 5 parts of chitin, 50 parts of the ionic liquid aqueous solution of 40-50% concentration;
The preparation method of carding agent:
(1)The ionic liquid aqueous solution for configuring 40-50% concentration, is warming up to 80 DEG C for ionic liquid aqueous solution, then by chitin
It is even added in ionic liquid aqueous solution, stirring and dissolving, mixing speed 600r/min, first is made in stirring and dissolving time 10min
Shell element-ionic liquid aqueous solution;
(2)Plant function extract particles mix with dehydrated alcohol to 70 DEG C of stirring and dissolvings of heating, stirring and dissolving time 40min,
Plant granule annex solution is made;
(3)By step(1)Chitin-the ionic liquid aqueous solution and step of preparation(2)The plant granule annex solution of preparation mixes,
50 DEG C are cooled to solution to stir evenly hereinafter, hemicellulase and sodium bicarbonate is added, and carding agent is made;Chitin takes off second
Acyl degree 96.5%, viscosity 700mPa.s, ignition residue 0.6%;Hemicellulase, enzyme activity storage rate 88.5%, enzyme activity are 1,000,000
U/g, effective component content 99.5%.
3, dissolution evaporation:Pretreated pulp is de- dry, it is ground into pulp particle, stabilizer, galla turcica is then added
Propyl propionate, NMMO solvent mix rising temperature for dissolving into cellulose solution;Cellulose solution is entered into cold boiler and carries out vacuum steaming
Hair forms spinning solution;
The additional amount of stabilizer is take off dry pulp quality 4.5%;Stabilizer is the mixing of azanol, tetrahydrofuran, Sodium Pyruvate
Object;In stabilizer, azanol, tetrahydrofuran, Sodium Pyruvate mass ratio be 6:25:2;
The additional amount of propylgallate is take off dry pulp quality 1.5%;
The mass fraction of over dry pulp is 80% after the de- dry pulp dregs of rice(Over dry pulp accounts for the quality percentage of de- dry rear pulp gross mass
Than);The not super more 8mm of partial size longest of the smashed pulp particle;
The concentration of NMMO solvent is 70%;The mass ratio of the de- dry pulp dregs of rice and NMMO solvent is 2:7;Warming temperature is 90 DEG C;
It is 115 DEG C that temperature, which is evaporated under reduced pressure, vacuum degree 14.6kpa.
4, spinning and post-processing:Manufactured spinning solution is entered filter to be filtered, removes impurity;Impurity is transferred to
Rinsing bowl carries out washing recovery section NMMO solvent, while filtered spinning solution and the plant function precursor liquid of preparation being pressed
According to 10:Enter spinning pump after 0.5 mass ratio mixing, functionality solvents then are made by spinning, post-processing and spin fiber
Cellulose fiber.
The component of plant function precursor liquid includes:
19 parts of filtered spinning solution, 0.15 part of propylgallate, 10 parts of plant function extract particles, mixed aid
0.3 part;Mixed aid is:Glycerol, dimethyl sulfoxide, Sodium Pyruvate mixture;Glycerol in mixed aid, dimethyl sulfoxide,
The mass ratio of Sodium Pyruvate is 5:1:0.5;
Plant function extract particles are:Saussurea involucrata extract, it is commercially available;200 mesh of plant function extract particles fineness, content of ashes
0.5%, moisture content 1%, total plate count 500cfu/g, content of beary metal 0.1ppm;
In spinning process, spinning speed 80m/min, air blowing temperature is 18 DEG C, air mass flow 50L/H, and blowing is opposite
Humidity is 35%;Spinning air gap 650mm;
Postprocessing working procedures include washing, oiling, drying, and remove bleaching process, further retain fiber strength, keep fiber original
Appearance.
50 DEG C of washing temperature;The finish that oils is Daikin production(DAIKIN), model TG-580S, finish uses dense
Degree is 25g/L, pH value 4;
Drying temperature is 130 DEG C.
Plant source modified cellulose fibre strength prepared by the present invention is high, has preferable wet modulus and elongation at break,
Fiber production process process stabilizing, in fiber end processing sequences, it is not easy to generate breakage phenomena, the characteristics of good spinnability,
Main indicator parameter is shown in Table 1
Table 1
As can be seen from Table 1, plant source modified cellulose fibre prepared by the present invention, doing breaking strength is 3.83-3.92 cN/
dtex;Wet breaking strength is 3.31-3.68 cN/dtex;Dry state modulus is 35.7-37.2;Hygrometric state modulus is 33.2-35.9;It says
Bright plant source modified cellulose fibre prepared by the present invention has good physical mechanical property and morphological stability.
In addition to this, plant source modified cellulose fibre prepared by the present invention, density with higher and lower water are swollen
Humidity and lower at yarn washing shrinkage, colludes with that breaking strength is higher, and specific Testing index is shown in Table 2
Table 2
As can be seen from Table 2, plant source modified cellulose fibre prepared by the present invention, density are 1.46-1.47 g.cm-3 ;Water
Peng Rundu is 52-55%;Yarn washing shrinkage is 0.5-0.7%;Colluding with breaking strength is 2.08-2.25 cN/dtex.
Plant source modified cellulose fibre density prepared by the present invention is larger, and water swelling capacity is smaller, illustrates preparation of the present invention
Fibre structure it is fine and close, influence of the variation of external environment to fibre morphology is smaller, further proves, fibre prepared by the present invention
Dimension, stable structure, therefore, in subsequent resultant yarn process or spinning process, all have good spinnability, made of knit
Object also has good deformation resistance.
For comprehensive detection as a result, from physical index, embodiment 2 is highly preferred embodiment of the present invention.
Comparative example 1
Pre-treatment step of the present invention is to objects such as the dry breaking strength of plant source modified cellulose fibre prepared by the present invention, dry state moulds
The method that Index Influence is larger, uses embodiment 2 below is managed, pre-treatment step of the invention is saved, then detects the plant of preparation
The index of correlation of material resource modified cellulose fibre;Specific Testing index is shown in Table 3
Table 3
As can be seen from Table 3, the plant source modified cellulose fibre prepared using the method for comparative example 1, Testing index and reality
It applies example 3 to compare, dry breaking strength, dry state modulus are colluded with breaking strength and all reduced significantly, and refer to other physics
Mark influences smaller.
Comparative example 2
In spinning of the present invention and post-processing step, the addition of plant function precursor liquid is fine to solvent-spun cellulose prepared by the present invention
The hygrometric state modulus and yarn washing shrinkage of dimension have large effect, and the method for using embodiment 2 below saves plant function of the invention
Plant function extract particles, are directly added in the spinning solution in spinning pump by the preparation of energy precursor liquid, and mixing is equal
It is even, then detect the index of correlation of the plant source modified cellulose fibre of preparation;Specifically it is shown in Table 4
Table 4
By table 4 it may be concluded that in spinning and post-processing step, the addition of plant function precursor liquid is to fibre prepared by the present invention
Density, wet breaking strength and the hygrometric state modulus of cellulose fiber have larger impact, therefore the preparation of the plant function precursor liquid is
An important inventive point of the invention.
Unless otherwise indicated, percentage employed in the present invention is weight percent, ratio of the present invention,
For mass ratio.
Finally it should be noted that:The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of plant source modified cellulose fibre, it is characterised in that:The preparation method of the fiber, including:Swelling, pretreatment
Step;The swelling step:Fiber pulp is immersed in deionized water, swelling is thoroughly mixed;The fiber of the pulp
Cellulose content >=96.5%, content of ashes≤0.06, small dust≤50mm2/ kg, dynamic viscosity 16.15-18.25mPa.s, the degree of polymerization
800 or less contents are less than 6%.
2. a kind of plant source modified cellulose fibre according to claim 1, it is characterised in that:The pre-treatment step:
Pulp after swelling is dehydrated within 20%, is then immersed pulp in pretreating agent, impregnating by pressure pretreatment, when pretreatment
Between be 30-50mn;The dosage of the pretreating agent is 3-10 times of pulp quality.
3. a kind of plant source modified cellulose fibre according to claim 1, it is characterised in that:The pretreated preparation
Method includes:The ionic liquid solution that concentration is 3-10% is warming up to 30-50 DEG C of temperature, pulp quality score 0.5-2% is added
Isomerous tridecanol stirs 5-10min, and carding agent is added, is again stirring for 5-10min, by being ultrasonically treated twice, must pre-process
Agent;The first time ultrasonic time 15-20min, supersonic frequency 150-180KHz;Second of ultrasonic time is 45-
60min, twice ultrasonic frequency are 100-120 KHz.
4. according to right to go 3 described in a kind of plant source modified cellulose fibre, it is characterised in that:The carding agent, by weight
Number meter is measured, includes following component, 1-2 parts of sodium bicarbonates, 0.2-0.5 parts of plant function extract particles, 3-10 parts of anhydrous second
Alcohol, 0.05-0.1 portions of hemicellulases, 1.5-5 parts of chitin, the ionic liquid aqueous solution of 20-50 parts of 40-50% concentration.
5. according to right to go 3 described in a kind of plant source modified cellulose fibre, it is characterised in that:The addition of the carding agent
Amount is the 10-30% of the pretreating agent quality.
6. according to right to go 3 described in a kind of plant source modified cellulose fibre, it is characterised in that:The preparation of the carding agent
Method includes:
(1)The ionic liquid aqueous solution for configuring 40-50% concentration, is warming up to 70-80 DEG C for ionic liquid aqueous solution, then by first
Shell element is even added in ionic liquid aqueous solution, stirring and dissolving, mixing speed 500-600r/min, stirring and dissolving time 5-
Chitin-ionic liquid aqueous solution is made in 10min;
(2)Plant function extract particles are mixed to 50-70 DEG C of stirring and dissolving of heating, stirring and dissolving time 30- with dehydrated alcohol
Plant granule annex solution is made in 40min;
(3)By step(1)Chitin-the ionic liquid aqueous solution and step of preparation(2)The plant granule annex solution of preparation mixes,
50 DEG C are cooled to hereinafter, addition hemicellulase and sodium bicarbonate stir evenly to solution.
7. according to right to go 6 described in a kind of plant source modified cellulose fibre, it is characterised in that:The chitin takes off second
Acyl degree >=96.5%, viscosity 550-700mPa.s, ignition residue≤0.6%;The hemicellulase, enzyme activity storage rate >=
88.5%, enzyme activity is ten thousand U/g of 95-100, effective component content >=99.5%.
8. a kind of plant source modified cellulose fibre according to claim 1, it is characterised in that:The preparation side of the fiber
Method further includes dissolution evaporation step;The dissolution evaporation step includes:Pretreated pulp is de- dry, it is micro- to be ground into pulp
Then stabilizer, propylgallate, NMMO solvent is added in grain, mix rising temperature for dissolving into cellulose solution;By cellulose solution
Be evaporated in vacuo into cold boiler and forms spinning solution;The additional amount of the stabilizer is the 2- for taking off dry pulp quality
4.5%。
9. a kind of plant source modified cellulose fibre according to claim 8, it is characterised in that:The stabilizer is hydroxyl
Amine, tetrahydrofuran, Sodium Pyruvate mixture;In the stabilizer, azanol, tetrahydrofuran, Sodium Pyruvate mass ratio be 5-
10:20-40:2-3。
10. a kind of plant source modified cellulose fibre according to claim 1, it is characterised in that:The preparation of the fiber
Method further includes spinning and post-processing step;The spinning and post-processing step:By manufactured spinning solution enter filter into
Row filtering, removes impurity;Impurity is transferred to rinsing bowl and carries out washing recovery section NMMO solvent, while filtered spinning is former
Liquid and the plant function precursor liquid of preparation are according to 10:Enter spinning pump after the mass ratio mixing of 0.5-1, then by spinning
Silk post-processes obtained functionality solvents spinning cellulose fibre;The component of the plant function precursor liquid includes:Filtered spinning
17-19 parts of stoste, 0.05-0.15 parts of propylgallate, 8-10 parts of plant function extract particles, mixed aid 0.1-0.3
Part.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810699421.6A CN108893796A (en) | 2018-06-29 | 2018-06-29 | A kind of plant source modified cellulose fibre |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810699421.6A CN108893796A (en) | 2018-06-29 | 2018-06-29 | A kind of plant source modified cellulose fibre |
Publications (1)
Publication Number | Publication Date |
---|---|
CN108893796A true CN108893796A (en) | 2018-11-27 |
Family
ID=64347335
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810699421.6A Pending CN108893796A (en) | 2018-06-29 | 2018-06-29 | A kind of plant source modified cellulose fibre |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108893796A (en) |
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109735951A (en) * | 2018-12-19 | 2019-05-10 | 中科纺织研究院(青岛)有限公司 | Compound ES fiber of a kind of seaweed modification and preparation method thereof |
CN111749010A (en) * | 2020-07-16 | 2020-10-09 | 宜宾惠美纤维新材料股份有限公司 | Peach blossom cellulose fiber and preparation process thereof |
CN112323503A (en) * | 2020-11-16 | 2021-02-05 | 浙江技立新材料股份有限公司 | Preparation method of macamide finishing agent for fabric finishing |
CN112680824A (en) * | 2020-12-24 | 2021-04-20 | 江苏盛恒化纤有限公司 | Preparation method of high-performance composite fiber |
CN113373689A (en) * | 2021-04-06 | 2021-09-10 | 百事基材料(青岛)股份有限公司 | Cotton macrofiber containing coffee active ingredient and preparation method thereof |
CN114059186A (en) * | 2021-11-04 | 2022-02-18 | 青岛邦特生态纺织科技有限公司 | Ginger extract fiber and preparation method thereof |
CN114710960A (en) * | 2019-10-15 | 2022-07-05 | 智能纤维股份公司 | Method for producing a cellulose functional fiber with high ion exchange capacity, cellulose functional fiber, textile product comprising cellulose functional fiber and clothing or furniture comprising cellulose functional fiber or textile product |
CN115300415A (en) * | 2022-09-15 | 2022-11-08 | 深圳前海港影生物科技有限公司 | Preparation method of carboxymethyl cellulose fiber mask |
CN115961368A (en) * | 2022-11-30 | 2023-04-14 | 新乡化纤股份有限公司 | Ionic liquid method fungus grass regenerated cellulose fiber and preparation method thereof |
CN116854996A (en) * | 2023-09-01 | 2023-10-10 | 保定天鹅新型纤维制造有限公司 | Cellulose mixed pulp and preparation method thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101476166A (en) * | 2009-01-13 | 2009-07-08 | 东华大学 | Improved preparation of cellulose spinning solution with ion liquid as solvent |
CN102080270A (en) * | 2010-12-21 | 2011-06-01 | 中原工学院 | Modification method of regenerated cellulose fibre |
CN102936762A (en) * | 2012-10-22 | 2013-02-20 | 中国纺织科学研究院 | Preparation method of chitosan/cellulose homogeneous spinning solution |
CN103556235A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Preparation technology of cellulose fiber spinning solution |
CN108004611A (en) * | 2017-11-30 | 2018-05-08 | 山东英利实业有限公司 | A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice |
-
2018
- 2018-06-29 CN CN201810699421.6A patent/CN108893796A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101476166A (en) * | 2009-01-13 | 2009-07-08 | 东华大学 | Improved preparation of cellulose spinning solution with ion liquid as solvent |
CN102080270A (en) * | 2010-12-21 | 2011-06-01 | 中原工学院 | Modification method of regenerated cellulose fibre |
CN102936762A (en) * | 2012-10-22 | 2013-02-20 | 中国纺织科学研究院 | Preparation method of chitosan/cellulose homogeneous spinning solution |
CN103556235A (en) * | 2013-10-28 | 2014-02-05 | 山东英利实业有限公司 | Preparation technology of cellulose fiber spinning solution |
CN108004611A (en) * | 2017-11-30 | 2018-05-08 | 山东英利实业有限公司 | A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109735951A (en) * | 2018-12-19 | 2019-05-10 | 中科纺织研究院(青岛)有限公司 | Compound ES fiber of a kind of seaweed modification and preparation method thereof |
CN114710960A (en) * | 2019-10-15 | 2022-07-05 | 智能纤维股份公司 | Method for producing a cellulose functional fiber with high ion exchange capacity, cellulose functional fiber, textile product comprising cellulose functional fiber and clothing or furniture comprising cellulose functional fiber or textile product |
CN111749010A (en) * | 2020-07-16 | 2020-10-09 | 宜宾惠美纤维新材料股份有限公司 | Peach blossom cellulose fiber and preparation process thereof |
CN112323503A (en) * | 2020-11-16 | 2021-02-05 | 浙江技立新材料股份有限公司 | Preparation method of macamide finishing agent for fabric finishing |
CN112680824A (en) * | 2020-12-24 | 2021-04-20 | 江苏盛恒化纤有限公司 | Preparation method of high-performance composite fiber |
CN113373689A (en) * | 2021-04-06 | 2021-09-10 | 百事基材料(青岛)股份有限公司 | Cotton macrofiber containing coffee active ingredient and preparation method thereof |
CN114059186A (en) * | 2021-11-04 | 2022-02-18 | 青岛邦特生态纺织科技有限公司 | Ginger extract fiber and preparation method thereof |
CN114059186B (en) * | 2021-11-04 | 2023-12-29 | 青岛邦特生态纺织科技有限公司 | Ginger extract fiber and preparation method thereof |
CN115300415A (en) * | 2022-09-15 | 2022-11-08 | 深圳前海港影生物科技有限公司 | Preparation method of carboxymethyl cellulose fiber mask |
CN115961368A (en) * | 2022-11-30 | 2023-04-14 | 新乡化纤股份有限公司 | Ionic liquid method fungus grass regenerated cellulose fiber and preparation method thereof |
CN115961368B (en) * | 2022-11-30 | 2023-09-12 | 新乡化纤股份有限公司 | Ionic liquid method fungus grass regenerated cellulose fiber and preparation method thereof |
CN116854996A (en) * | 2023-09-01 | 2023-10-10 | 保定天鹅新型纤维制造有限公司 | Cellulose mixed pulp and preparation method thereof |
CN116854996B (en) * | 2023-09-01 | 2023-11-03 | 保定天鹅新型纤维制造有限公司 | Cellulose mixed pulp and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108893796A (en) | A kind of plant source modified cellulose fibre | |
CN101694019B (en) | Solvent method high-wet-modulus bamboo fiber and preparation method thereof | |
CN101089249A (en) | Preparation and application of cellulose mixed fibre using ion liquid as solvent | |
CN101230493A (en) | Solvent preparation cellulose bamboo charcoal fibre and use thereof | |
CN109234826B (en) | Method for preparing lyocell fibers by using bamboo as raw material | |
CN104004207B (en) | Ionic liquid prepares corn cob fiber cellulosic material or the method for blended fiber material | |
CN101225552A (en) | Method for dissolving and processing wood/cotton bamboo hemp fibre by employing ionic liquid | |
CN101220523A (en) | Method for manufacturing cellulose fibroin composite fiber by using solvent method | |
CN101240454A (en) | Solvent method for preparing cellulose mixing fibre and application thereof | |
CN107988652A (en) | A kind of composite fibre and preparation method comprising Lotus Leafextract and Semen Nelumbinis extract | |
CN101230494A (en) | Solvent preparation cellulose blending fibre and use thereof | |
CN100503907C (en) | Method for direct manufacturing regenerated bamboo fiber from papermaking-level bamboo pulp dregs | |
CN105671663B (en) | A kind of preparation method and applications of nettle extract protein compound additive | |
CN111394817A (en) | Novel preparation process of regenerated cellulose fiber | |
CN112538663A (en) | Lyocell fiber, Lyocell fiber mask cloth and manufacturing method thereof | |
CN113242894B (en) | Separation of fibers | |
CN103556248A (en) | Bamboo charcoal Lyocell fiber and preparation process thereof | |
CN101089250A (en) | Preparation and application of bamboo pulp fibre using ion liquid as solvent | |
CN1129680C (en) | Process for production of LYOCELL fiber with bamboo material | |
CN101768790B (en) | Sheath core composite fibre of chitin and cellulose and preparation method thereof | |
CN109234828A (en) | A kind of solvent method high-wet-modulus cotton fiber and preparation method thereof | |
CN108486673A (en) | Regenerated celulose fibre and preparation method thereof containing binchotan | |
CN111826722A (en) | Preparation method of impregnated powder and dried lyocell fiber | |
CN101225553A (en) | Method for dissolving and processing ceiba bamboo hemp fibre by employing ionic liquid | |
CN105113035B (en) | Regenerated fiber and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181127 |