CN106435760B - A kind of fine design method of apocynum fibre - Google Patents

A kind of fine design method of apocynum fibre Download PDF

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Publication number
CN106435760B
CN106435760B CN201610969347.6A CN201610969347A CN106435760B CN 106435760 B CN106435760 B CN 106435760B CN 201610969347 A CN201610969347 A CN 201610969347A CN 106435760 B CN106435760 B CN 106435760B
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bluish dogbane
dogbane bast
bast
apocynum fibre
degumming
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CN106435760A (en
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张元明
韩光亭
张玉清
王聪儿
孙婷婷
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Shandong Hengfeng New Yarn And Fabric Innovation Center Co ltd
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Qingdao University
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01CCHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
    • D01C1/00Treatment of vegetable material
    • D01C1/02Treatment of vegetable material by chemical methods to obtain bast fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/02Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06CFINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00Heating or cooling textile fabrics
    • D06C7/04Carbonising or oxidising

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Molecular Biology (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses the infiltrations of a kind of fine design method of apocynum fibre, including bluish dogbane bast to activate, beats cake dress cage, directional catalyzing oxidation, chemical Degumming and post-processing step;After it uses organic amine solvent to carry out infiltration activation to bluish dogbane bast, catalytic oxidation treatment is oriented to lignin, pectin and hemicellulose using ferrous salt solution and activator;And it is organically combined by the way that the series techniques means such as activation process and directional catalyzing oxidation will be infiltrated, so that the fine design method of the apocynum fibre of the present invention, the features such as indexs such as, the apocynum fibre finish fineness, length, the intensity that are obtained good with degumming effect are good, quality is excellent, good spinnability;Also, chemical cost amount is small in process, environmental protection pressure is small, and technology controlling and process is simple;The utility consumptions such as water power vapour are small, efficient, are suitable for industrialized production.

Description

A kind of fine design method of apocynum fibre
Technical field
The present invention relates to a kind of processing method of flaxen fiber more particularly to a kind of fine design sides of apocynum fibre Method.
Background technology
Bluish dogbane also known as wild flax, wartwort fiber crops, red building, apocynum cannabinum etc., are a kind of perennial herb plants, are belonged to Apocynaceae, is widely distributed in the northern area in China, and Tarimhe River and Kongquehe of the integrated distribution in Xinjiang are littoral, because its It spreads out Plain growth and most contains and gain the name in Xinjiang.There are many excellent characteristic, soft and good lusters to have silk for apocynum fibre Gloss, numb very light, the softness of cotton, the malleability of suede, and have pharmacological action is once described as by crudefiber crop expert Feng Yunhe etc. " wild The king of fiber ", therefore it is acknowledged as ideal textile fabric.
Apocynum fibre is a kind of bast fiber, it is located in the phloem tissue on bluish dogbane plant stem, is in fibre bundle Shape, individuals fibers individualism.Bluish dogbane single fiber is that a kind of two end seal closes among ﹑ have thick in the middle part of born of the same parents' chamber ﹑ and both ends thin thin Born of the same parents' shape object, section are in apparent irregular kidney-shaped, and lumen is smaller, and fiber is longitudinal without torsion, and surface is there are many vertical line and has Horizontal section exists.Fibre fineness is about 3~4dtex, and length is 20~25mm, and fiber width is 10~50 μm.
The chemical composition of bluish dogbane bast has certain difference with other bast-fibres.Bluish dogbane bast hemicellulose level 16.31%, content of lignin 12.09% is above Zhu Ma ﹑ Ya Ma ﹑ hemps, especially content of lignin and is apparently higher than other fiber crops Class, and it is minimum in all bast-fibres that content of cellulose, which is only 45.74%,.
Since bluish dogbane bast non-cellulose components are high, up to nearly the 55% of bluish dogbane bast, especially hemicellulose and Content of lignin is high, is more than the 28% of bluish dogbane bast.Therefore, the more other bast-fibres of apocynum degumming are more difficult, tradition Bast-fibre Degumming method be not appropriate for the degumming process of apocynum fibre, it is necessary to select to take off in conjunction with bluish dogbane own characteristic Gluing method and technique.
In the prior art, common apocynum fibre Degumming method is main or the chemical method of traditional bast-fibre degumming, Bioanalysis or Physical.Wherein, for chemical method because using a large amount of chemical reagent that waste water is caused to be difficult to handle, environmental pollution is serious, takes off Hot conditions energy consumption cost needed for glue is high, while chemical Degumming is difficult between Proper Match fibre strength, length and fineness Relationship, degumming excessively leads to a large amount of short flannels and fibre strength is low, and then fiber residual gum content is high on the contrary, especially lignin residue amount Height causes fiber thick and stiff, and flexible small, the limit count of obvolvent force difference, yarn is low, and wiriness, filoplume is more, and prodding and itching feeling is strong, The excellent performance of apocynum fibre cannot be fully demonstrated, the application range of apocynum fibre is seriously limited.
For bioanalysis, many bioenzyme activities are insufficient, be generally difficult to be applied to apocynum fibre internal component it is complicated, Compact structure part is especially difficult to removal lignin portion, therefore that there are degumming qualities is unstable, efficiency is low, consumption for bioanalysis Duration, it is of high cost the problems such as, be largely required for chemical method to make up the deficiency of its degumming technology.
Physical Degumming method includes ultrasonication method, microwave treatment method and steam explosion etc., wherein application is the most general It is steam explosion technology all over be.But in the steam explosion processing procedure in relation to research report, vapor (steam) temperature is high, pressure is big, In particular, generally requiring multiple repetition exploding technology, inevitably, apocynum fibre strength damage and fiber will be caused long Degree loss.
In short, for the high feature of lignin in bluish dogbane bast raw material and hemicellulose level, not to bluish dogbane Raw material carry out it is pretreated in the case of, when by single chemistry, biological or physics effect degumming, processing conditions is difficult to Control, fibre strength is difficult to rationally control with length, fineness relationship, otherwise apocynum fibre obtained by processing it is thick, it is hard, rough or Fiber strength is low, cast tow rate is high, seriously affects bluish dogbane product quality.
In order to improve apocynum fibre performance, it is promoted to efficiently use, both at home and abroad to sieve on the basis of traditional Degumming method Cloth flaxen fiber fine techniques have also carried out a few thing, but are the soft treatment for the softening and textile for concentrating on fiber mostly, Fining without solving the problems, such as fiber itself, only softening fibre and reduce fibre-fibre friction power, this is obviously to bluish dogbane Product is lightening and superior has little significance.
The fiber fine design method of low damage is the key that promote apocynum fibre fiber utilization value, represents The development trend of industry technology and direction.
Invention content
It is an object of the present invention to provide a kind of fine design methods of apocynum fibre, to overcome the de- of the prior art The apocynum fibre that time-consuming for gluing method generally existing, chemicals usage amount is big, prepared is short, thick, hard, low strength Etc. technical problems.
Present invention technical solution used for the above purpose is a kind of fine design side of apocynum fibre Method, which is characterized in that include the following steps:
The first step, the infiltration activation step of bluish dogbane bast
Bluish dogbane bast is placed in vapor tight tank, it is molten to be immersed in the organic amine that mass percent concentration is 40%~60% In agent, it is continuously stirred at room temperature 12~20 hours, so that bluish dogbane bast fully infiltrates activation, it then, will be organic in tank Amine solvent is vented, and takes out the bluish dogbane bast by infiltration activation, spare;
Second step beats cake dress cage step
By in the numb cage of bluish dogbane bast feeding by infiltration activation, cake is beaten using pancake making machine;When feeding, numb cage is with 3~5 Rev/min speed do not stop to rotate, pancake making machine machinery foot up and down motion beat reality beats bluish dogbane bast;Meanwhile sprinkle water duckbilled from Up to lower elution of continuously spraying water into numb cage, elution water temperature is 50 DEG C~80 DEG C;
Third walks, directional catalyzing oxidation step
It will be after playing cake processing, the numb cage for being loaded with bluish dogbane bast is integrally placed in glue kettle, is opened liquid feed valve, is made Ferrous salt solution to liquid level is first injected into glue kettle with high-pressure pump did not had bluish dogbane bast;
Then, continue to keep high-pressure pump operating, so that ferrous salt solution is followed with external ferrous salt solution pressure in glue kettle Ring, keep glue kettle in ferrous salt solution always with swiftly flowing state constant impingement bluish dogbane bast 15~30 minutes after, Stop high-pressure pump, close liquid feed valve, open liquid valve, liquid valve will be closed after the ferrous salt solution emptying in glue kettle;
Then, liquid feed valve is opened, activator bath foam to liquid level is first injected into glue kettle using high-pressure pump did not had bluish dogbane Bast;Then, continue to keep high-pressure pump operating, so that activator bath foam and external activator bath foam forced circulation in glue kettle, Activator bath foam in glue kettle is kept to stop height after 1~2 hour always with swiftly flowing state constant impingement bluish dogbane bast Press pump closes liquid feed valve, opens liquid valve, will close liquid valve after the activator bath foam emptying in glue kettle;
Above-mentioned activator is H2O2, Peracetic acid or carbamide peroxide solution;
4th step, chemical Degumming step
Liquid feed valve is opened, alkaline degumming liquid is pumped into glue kettle, until liquid level did not had bluish dogbane bast, heating to boil, and Continuously cooking 0.5~2 hour under fluidized state;
Then, degumming liquid is emptied, sulfuric acid bath foam is injected or hydrochloric acid bath foam washs bluish dogbane bast to pH value≤7;Make again With clear water rinsed clean repeatedly, apocynum fibre semi-finished product are obtained;
5th step, post-processing step
By obtained apocynum fibre semi-finished product successively through being dehydrated, oiling, dry to get apocynum fibre finished product.
Preferably, above-mentioned organic amine solvent be ethylenediamine, dimethylformamide or dimethylacetylamide in one kind or It is several.
Further preferably, above-mentioned ferrous salt solution is FeSO4Solution or FeCl2Solution, mass percent concentration are 0.03%~1%.
Further preferably, the mass percent concentration 0.5%~2.5% of above-mentioned activator bath foam, pH value are 3~5, temperature It is 30 DEG C~50 DEG C;Bath raio is 1:10.
Further preferably, above-mentioned alkaline degumming liquid is the sodium hydroxide solution that mass percent concentration is 0.1%~1%;
The mass percent concentration of the sulfuric acid or hydrochloric acid bath foam is 0.1%, bath raio 1:20.
Further preferably, the fine design method of above-mentioned apocynum fibre, which is characterized in that obtained bluish dogbane The fineness of fibrous finished product is 3.2~4.5dtex, and residual gum content is 3.68%~5.22%, and fibre strength is 3.8~7.6cN/ The average length of dtex, fiber are more than 35mm.
The technical effect brought directely by the technical proposal is that degumming effect good (residual gum content is 3.68%~5.22%), Obtained apocynum fibre finish fineness thin (for 3.2~4.5dtex), fibre strength index are good (for 3.8~7.6cN/ Dtex), fabric is (average length is more than 35mm) of fine quality.
The fine design method of the apocynum fibre of above-mentioned technical proposal, in entire production process, chemical cost amount Small, environmental protection pressure mitigates, and technique controlling difficulty is greatly reduced;The utility consumptions such as water power vapour are small, production efficiency is high, production It is at low cost.
To more fully understand the technical characterstic of the present invention, shows detailed analysis and be described as follows:
In above-mentioned technical proposal, bluish dogbane bast raw material is placed in organic amine solvent, and is impregnated under oscillation, is obtained Sufficient activation process, raw material become fluffy, soft (this is because under the action of organic amine, in bluish dogbane bast raw material Hydrogen bond is destroyed, and the colloids such as lignin, hemicellulose, pectin and the combination of colloid and colloid and cellulose weaken, and structure becomes It is loose, while the amorphous region of cellulose increased and by swollen), while the activation process through organic amine, it can reduce final The rigidity of keen-witted and capable gunny products, promotes its flexibility, can textile processibility and comfort.
In above-mentioned technical proposal, beat during cake using while beat cake, while hot water spray method, to infiltrated activation process Bluish dogbane bast carry out beat cake, the colloid in bluish dogbane bast can be made further to soften under the action of soaking of warm water, and It is partly removed under the action of mechanical force;Especially, it beats during cake due to mechanical external force effect and warm water processing effect, it can be effective Removal subsequent handling is difficult to the part bluish dogbane bast surface layer sclerderm removed, and then it is strong that following process processing can be greatly reduced The consumption of degree and chemical reagent.
It is important to note that in above-mentioned technical proposal, in directional catalyzing oxidation process, sieve after infiltrated activation Under the action of cloth fiber crops bast is due to organic amine, hydrogen bond is destroyed in bluish dogbane bast raw material, lignin, hemicellulose, pectin etc. Colloid and the combination of colloid and colloid and cellulose weaken, and structure becomes loose, and hemicellulose, pectin and the lignin on surface exist It is adsorbed under the action of oxygen-containing group and under the action of organic amine infiltrates the nitrogen-containing group for the organic amine brought into activation process More Fe2+
After activator is added, it is adsorbed with Fe2+Hemicellulose, pectin and lignin take the lead in by oxidative degradation, partly by oxygen Change is degraded to small organic molecule and directly dissolves removal, is partly oxidized to the substance that subsequent chemistry degumming is more easy to removal.
In directional catalyzing oxidation step, Fe is adsorbed2+Bluish dogbane bast be placed directly within containing activator without washing Solution in, it is therefore an objective to protect Fe2+Directional catalyzing activator decomposes, and then oxidative lignin, pectin and hemicellulose, enhancing are urged Change oxidation effectiveness.
Wherein, Activation Activation and Fe are infiltrated using organic amine2+Ion and hydrogen peroxide (or Peracetic acid or carbamide peroxide Solution) it impregnates one of the key problem in technology point that catalytic oxidation treatment is the present invention is oriented to bluish dogbane bast, to final sieve Cloth flaxen fiber treatment effect plays very crucial effect.The reason is as follows that:
In bluish dogbane bast, apocynum fibre cellulose fiber is made in bonding for the colloids such as pectin, hemicellulose and lignin With lower bunchy (technique) fiber, wherein single fiber length is 20~25mm, and diameter is then 10~50 μm, colloid (pectin, hemicellulose Element, lignin etc.) it is connected with each other by hydrogen bond, covalent bond, van der Waals interaction with cellulose, these gum dispersions are in the fibre Between or be enclosed in outside fiber, form fine and close Network Three-dimensional space structure so that cellulosic sections are not easy to disperse.Traditional is de- Gluing method is all the effect by chemical reagent or biological enzyme, from outside to inside successively strips down the colloid in bundle fiber, is caused Keep degumming degree inside and outside raw material inconsistent, outer layer degumming degree is better than internal layer, leads to end article quality decline, while this process Reaction condition is not easy to control, if degumming effect is violent, fiber can be caused to shorten, lose weaving use value;If degumming effect It is bad, residual gum content is higher, and fiber will be caused thick, hard, rough, be equally unfavorable for subsequent textile process process and use.
Therefore, the degumming mode for successively removing colloid from outside to inside to change, with condition Proper Match sieve of milder Relationship between cloth fiber crops process of fiber intensity, fineness, length needs the orientation removal that part non-cellulosic material is carried out to raw material.
And the organic amine activating pretreatment of above-mentioned technical proposal, it is not destroy apocynum fibre bulk composition cellulose poly- In the case of right, interior the component molecules such as lignin, hemicellulose, pectin in raw material and intermolecular and lignin, partly are destroyed Hydrogen bond between cellulose, pectin and cellulosic molecule, reduction colloid and colloid and the binding force of colloid and cellulose, increase simultaneously Add the swollen degree of raw material, partial removal hemicellulose, pectin and lignin are conducive to the infiltration of follow-up degumming reagent and further It has an effect.Meanwhile using organic amine as infiltration activating reagent, on the one hand can also acting on increase with lignin, it is water-soluble, On the other hand have the brilliant effect that disappears, material crystal degree can be reduced, increase amorphous region area, improve raw material hydrophily, therefore, It is more advantageous to the difficulty for further decreasing follow-up degumming.
What is more important, under the action of organic amine, lignin, pectin, hemicellulose etc. in bluish dogbane bast raw material The destruction of hydrogen bond, colloid and colloid between component molecules are interior and intermolecular and lignin, hemicellulose, pectin and cellulosic molecule And the decrease of colloid and cellulose binding force, the increase of raw material swollen degree, so that the tough skin structure of bluish dogbane is become loose, in turn Keep raw material specific surface area increased simultaneously as the colloids such as hemicellulose, pectin and lignin are wrapped in fibrous outer, because herein Hemicellulose, pectin and content of lignin in raw material surface increase, and so that more groups containing O is exposed to raw material surface, in half fiber Under the action of dimension element, pectin and lignin electron-donating group containing O, more Fe can be effectively adsorbed2+Ion enhances bluish dogbane bast Raw material Fe2+The activity of ionic adsorption, while in organic amine infiltrates activation process, organic amine can be brought into bluish dogbane bast raw material Substance, the nitrogen-containing group in organic amine can also enhance bluish dogbane bast raw material Fe2+The activity of ionic adsorption is conducive to follow-up orientation and lives Fe during change2+The absorption of ion, and then be conducive to the progress of follow-up directional catalyzing oxidation.
In directional catalyzing oxidation process, the bluish dogbane raw material of infiltrated activation process, due to hemicellulose, pectin and wood Quality Surface oxygen-containing groups increase and the introducing of nitrogen-containing group, in FeSO4、FeCl2Or (NH4)Fe(SO4)2The immersion of solution Under, Fe is largely adsorbed on bluish dogbane raw material surface2+, then in hydrogen peroxide or Peracetic acid or carbamide peroxide solution treatment, half The Fe of cellulose, pectin and lignin absorption2+In the H that hemicellulose, pectin and lignin surface catalysis directly add2O2Or mistake The H that fluoroacetic acid or the hydrolysis of carbamide peroxide solution generate2O2It decomposes, in acid condition, Fe2+It is catalyzed H2O2It decomposes and generates oxidation Very competent HO, since the extremely strong HO of the oxidability of generation is predominantly located at hemicellulose, pectin and lignin surface, Therefore part hemicellulose and pectin can be degraded to water soluble small organic molecule and are dissolved in the water;Simultaneously because HO oxidabilities are extremely strong, can will be complicated and be difficult to the lignin side chain C-C keys removed fracture or ring-opening reaction occurs, it is raw It is more easy to the structure of removal at subsequent chemistry degumming, is easy to follow-up degumming removal.HO oxidation radius very littles simultaneously, and due to Cellulose is wrapped in hemicellulose, pectin and lignin, therefore the oxidation of HO is difficult to that cellulose oxidation is made to degrade.
During chemical Degumming, high temperature alkaline solution can hydrolyze the remaining most non-cellulosic material of removal, especially may be used Make the lignin that oxidized rear side chain C-C keys were broken or occurred ring-opening reaction that hydrolysis occur and remove so that fiber is into one Step dispersion, while cellulose disappears brilliant effect under lye, reduction crystallinity improves the hydrophily of fiber, softening fibre.
In above-mentioned technical proposal, the bluish dogbane bast raw material after infiltrating activating pretreatment is directly set without washing It carries out buying cake in pancake making machine.Main cause has neither part nor lot in the organic amine of priming reaction further to sieve first, during buying cake Cloth fiber crops bast is activated, second is that in order to which effective protection organic amine is to the activation effect of bluish dogbane bast raw material.
In above-mentioned technical proposal, break the bluish dogbane bast raw material after cake, without washing, that is, be directly injected into ferrous salt solution into Row processing, main cause is the remaining organic amine reagent not yet completely removed during buying cake, and former with apocynum fibre Expect the organic amine reagent chemically reacted, more Fe can be adsorbed under the left and right for the N element that organic amine itself contains2+, increase Strong catalytic oxidation effect.
In above-mentioned technical proposal, why the bluish dogbane bast raw material by directional catalyzing oxidation is existed without washing After emptying reaction solution, it is pumped directly into lye and carries out degumming process, it is therefore intended that, when, wherein remaining undecomposed activator can To increase the degumming effect and bleaching effect in soda boiling scouring processes, second is that, remaining Fe2+It is de- coagulation can be carried out to degumming liquid Color mitigates subsequent wastewater treatment difficulty.
Certainly, correspondingly, compared with the processing of the pre-sour of the prior art, pre- alkali process, pre- urine oxygen processing chemical Degumming method, Before chemical Degumming, a water-washing step is omitted, reduces water consume.
In addition, compared with existing biology, chemical Degumming technology, this technology is due to remaining Fe2+Ion is in chemical Degumming mistake There is coagulation decoloration effect in journey, the coloring matter in effluent part can be taken off.Therefore, to generated during subsequent production Waste water decoloring intractability accordingly reduces.
Meanwhile with the chemical Degumming method of prior art ratio, above-mentioned technical proposal needs not move through the length of a large amount of chemical reagent Time boiling, by Fe under organic amine infiltration activation and acid condition2+The selective paraffin oxidation for the HO that ionic catalysis activator generates Degradation, which carries out apocynum fibre degumming, has the significant advantages such as efficient, pollution is small.
In above-mentioned technical proposal, pickling prevents alkali to cellulose into one then in order to neutralize the alkaline reagent of chemical Degumming Step degradation;The surface state for oiling to improve fiber, increases the laxity and softness of fiber, convenient for follow-up spinning.
In short, just because of the combination of above-mentioned series technique means so that in apocynum fibre crude product alkaline boiling, Compared with the prior art boiling handle, the time required to chemical levels, boiling in terms of be greatly decreased or save, this is for having Effect mitigates damage of the alkaline scouring process to fibrous physics index, reduces wastewater treatment difficulty, alleviates environmental protection pressure, improves production effect Rate reduces production cost and all has apparent positive effect.
Supplementary explanation:In above-mentioned technical proposal, by alkaline scouring treated apocynum fibre, remaining colloid in fiber And pigment, it is further removed, to reach ideal flax fiber separation index and whiteness index.
In conclusion the present invention compared with the existing technology, has the advantages that:
1, it on the basis of obtaining compared with the better degumming effect of the prior art (residual gum content is 3.68%~5.22%), is obtained Apocynum fibre finish fineness thin (for 3.2~4.5dtex), fibre strength index good (for 3.8~7.6cN/dtex), the fibre obtained Tie up average length length (average length is more than 35mm), good spinnability;
2, chemical cost amount is small, environmental protection pressure mitigates, and technique controlling difficulty is greatly reduced;
3, the utility consumptions such as water, electricity, vapour are small, improve production efficiency, reduce production cost.
Specific implementation mode
With reference to embodiment, the present invention is described in detail.
Embodiment 1
The bluish dogbane bast places of origin of raw materials:Xinjiang
Processing method is as follows:
Bluish dogbane bast is placed in vapor tight tank, is immersed in the ethylenediamine that mass percent concentration is 40%, in room temperature It persistently stirs 12 hours down, so that bluish dogbane bast fully infiltrates activation, then, the ethylenediamine in tank is vented, takes out and passes through Infiltrate the bluish dogbane bast of activation.
Then it carries out buying cake, bluish dogbane bast obtained by cake will be beaten and numb cage is placed in glue kettle together, be pumped into quality percentage The FeSO that specific concentration is 0.05%4Solution, until do not cross bluish dogbane bast makes FeSO using high-pressure pump at room temperature4Inside and outside solution Cycle 15 minutes empties FeSO4After solution, it is pumped into the hydrogen peroxide solution that mass percent concentration is 0.5%, at 30 DEG C of cycles Reason 1 hour after emptying hydrogen peroxide solution, is pumped into the sodium hydroxide solution that mass percent concentration is 0.1%, and boiling is boiled 1 hour.
Then, pickling is carried out at room temperature to the fiber after boiling, pickle is the sulphur that mass percent concentration is 0.1% (acid cleaning process selects bath raio for 1 for acid or solution:20), pickling time is 5 minutes.
It is neutrality by fiber washing to pH value, finally, successively to get fine bluish dogbane fibre after being dehydrated, oiling, dry Dimension.
Examination and test of products testing result:
Obtained apocynum fibre residual gum content is 5.22%, and average fiber length is more than 35mm, and fibre strength is 7.6cN/dtex, fibre fineness 4.5dtex.
Embodiment 2
The bluish dogbane bast places of origin of raw materials:Xinjiang
Processing method is as follows:
Bluish dogbane bast is placed in vapor tight tank, is immersed in the dimethylformamide that mass percent concentration is 60%, It is continuously stirred at room temperature 20 hours, so that bluish dogbane bast fully infiltrates activation, then, the dimethylformamide in tank is put Sky takes out the bluish dogbane bast by infiltration activation.
Then it carries out buying cake, bluish dogbane bast obtained by cake will be beaten and numb cage is placed in glue kettle together, be pumped into quality percentage The FeCl that specific concentration is 0.1%2Solution, until do not cross bluish dogbane bast makes FeCl using high-pressure pump at room temperature2It is followed inside and outside solution Ring 30 minutes empties FeCl2After solution, it is pumped into the peracetic acid soln that mass percent concentration is 2.5%, at 50 DEG C of cycles Reason 1 hour after emptying peracetic acid soln, is pumped into the sodium hydroxide solution that mass percent concentration is 0.1%, it is small that boiling boils 0.5 When.
Then, pickling is carried out at room temperature to the fiber after boiling, pickle is the salt that mass percent concentration is 0.1% (acid cleaning process selects bath raio for 1 to acid solution:20), pickling time is 5 minutes.
It is neutrality by fiber washing to pH value, finally, successively to get fine bluish dogbane fibre after being dehydrated, oiling, dry Dimension.
Examination and test of products testing result:
Obtained apocynum fibre residual gum content is 3.68%, and average fiber length is more than 35mm, and fibre strength is 3.8cN/dtex, fibre fineness 3.2dtex.
Embodiment 3
The bluish dogbane bast places of origin of raw materials:Xinjiang
Processing method:Except FeSO4Solution quality percent concentration is 1%, the time of alkaline degumming liquid continuously cooking is 2 small When, use carbamide peroxide solution substitute hydrogen peroxide, use mass percent concentration to replace matter by 50% dimethylacetylamide The ethylenediamine that percent concentration is 40% is measured, the mass percent concentration of carbamide peroxide Solutions Solution is except 1.5%;
Remaining, with embodiment 1.
Examination and test of products testing result:
Obtained apocynum fibre residual gum content is 4.62%, and average fiber length is more than 35mm, and fibre strength is 6.1cN/dtex, fibre fineness 3.9dtex.
It should be noted that organic amine solvent used in the present invention can also be ethylenediamine, dimethylformamide or The mixture of mixing or three two-by-two of dimethylacetylamide.

Claims (6)

1. a kind of fine design method of apocynum fibre, which is characterized in that include the following steps:
The first step, the infiltration activation step of bluish dogbane bast
Bluish dogbane bast is placed in vapor tight tank, the organic amine solvent that mass percent concentration is 40%~60% is immersed in In, it is continuously stirred at room temperature 12~20 hours, so that bluish dogbane bast fully infiltrates activation, then, by the organic amine in tank Class solvent vent takes out the bluish dogbane bast by infiltration activation, spare;
Second step beats cake dress cage step
By in the numb cage of bluish dogbane bast feeding by infiltration activation, cake is beaten using pancake making machine;When feeding, numb cage with 3~5 turns/ The speed of minute does not stop to rotate, and the up and down motion of pancake making machine machinery foot is beaten beats bluish dogbane bast in fact;Meanwhile sprinkle water duckbilled from up to It continuously sprays water down and elutes into numb cage, elution water temperature is 50 DEG C~80 DEG C;
Third walks, directional catalyzing oxidation step
It will be after playing cake processing, the numb cage for being loaded with bluish dogbane bast is integrally placed in glue kettle, is opened liquid feed valve, is used height Press pump first injects ferrous salt solution to liquid level into glue kettle and did not had bluish dogbane bast;
Then, continue to keep high-pressure pump operating, so that ferrous salt solution and external ferrous salt solution forced circulation in glue kettle, are protected Hold in glue kettle ferrous salt solution always with swiftly flowing state constant impingement bluish dogbane bast 15~30 minutes after, stop high pressure Pump closes liquid feed valve, opens liquid valve, will close liquid valve after the ferrous salt solution emptying in glue kettle;
Then, liquid feed valve is opened, activator bath foam to liquid level is first injected into glue kettle using high-pressure pump did not had bluish dogbane bast; Then, continue to keep high-pressure pump operating, so that activator bath foam and external activator bath foam forced circulation in glue kettle, keep de- Activator bath foam is always with swiftly flowing state constant impingement bluish dogbane bast in glue tank, after 1~2 hour, stops high-pressure pump, closes It closes liquid feed valve, open liquid valve, liquid valve will be closed after the activator bath foam emptying in glue kettle;
Above-mentioned activator is H2O2, Peracetic acid or carbamide peroxide solution;
4th step, chemical Degumming step
Liquid feed valve is opened, alkaline degumming liquid is pumped into glue kettle, until liquid level did not had bluish dogbane bast, heating to boil, and is being boiled Rise continuously cooking 0.5~2 hour under state;
Then, degumming liquid is emptied, sulfuric acid bath foam is injected or hydrochloric acid bath foam washs bluish dogbane bast to pH value≤7;It reuses clear Water rinsed clean repeatedly, obtains apocynum fibre semi-finished product;
5th step, post-processing step
By obtained apocynum fibre semi-finished product successively through being dehydrated, oiling, dry to get apocynum fibre finished product.
2. the fine design method of apocynum fibre according to claim 1, which is characterized in that the organic amine is molten Agent is one or more of ethylenediamine, dimethylformamide or dimethylacetylamide.
3. the fine design method of apocynum fibre according to claim 1, which is characterized in that the ferrous salt solution For FeSO4Solution or FeCl2Solution, mass percent concentration are 0.03%~1%.
4. the fine design method of apocynum fibre according to claim 1, which is characterized in that the activator bath foam Mass percent concentration be 0.5%~2.5%, pH value be 3~5, temperature be 30 DEG C~50 DEG C;Bath raio is 1 ︰ 10.
5. according to the fine design method of any apocynum fibres of claim 1-4, which is characterized in that the alkalinity Degumming liquid is the sodium hydroxide solution that mass percent concentration is 0.1%~1%;
The mass percent concentration of the sulfuric acid bath foam or hydrochloric acid bath foam is 0.1%, and bath raio is 1 ︰ 20.
6. according to the fine design method of any apocynum fibres of claim 1-4, which is characterized in that obtained 3.2~4.5dtex of fineness of apocynum fibre finished product, residual gum content are 3.68%~5.22%, and fibre strength is 3.8~7.6cN/ The average length of dtex, fiber are more than 35mm.
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