CN106319642A - Refining processing method for apocynum venetum fiber - Google Patents

Refining processing method for apocynum venetum fiber Download PDF

Info

Publication number
CN106319642A
CN106319642A CN201610953766.0A CN201610953766A CN106319642A CN 106319642 A CN106319642 A CN 106319642A CN 201610953766 A CN201610953766 A CN 201610953766A CN 106319642 A CN106319642 A CN 106319642A
Authority
CN
China
Prior art keywords
apocyni veneti
herba apocyni
bast
degumming
activation
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.)
Granted
Application number
CN201610953766.0A
Other languages
Chinese (zh)
Other versions
CN106319642B (en
Inventor
张元明
韩光亭
徐颖
徐维敬
李洋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Qingdao University
Original Assignee
Qingdao University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Qingdao University filed Critical Qingdao University
Priority to CN201610953766.0A priority Critical patent/CN106319642B/en
Publication of CN106319642A publication Critical patent/CN106319642A/en
Application granted granted Critical
Publication of CN106319642B publication Critical patent/CN106319642B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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

Landscapes

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

Abstract

The invention discloses a refining processing method for an apocynum venetum fiber. The method comprises the steps of infiltrating and activating apocynum venetum bast; performing steam explosion activating treatment; caking and putting into a cage; performing directional catalytic oxidizing; chemically degumming and post-processing. Organic amine is adopted for infiltrating and activating and steam explosion activating treatment is performed, and then a ferrite solution and an activating agent are adopted for performing directional catalytic oxidization on lignin and hemicellulose; through the organic combination of a series of technical methods, such as, infiltration and activation, steam explosion, degumming and directional catalytic oxidization, the production method provided by the invention has the characteristics of good degumming effect, excellent indexes including finish fineness, length, strength and the like of the acquired apocynum venetum fiber, high quality, excellent spinning property, and the like; the chemical consumption is low; the environment-friendly pressure is low; the technical control is simple; the consumption of the public works, such as water, electricity and gas, is low, the efficiency is high and the method is suitable for industrial production.

Description

A kind of fine design method of Herba Apocyni veneti degummed ramie
Technical field
The processing method that the present invention relates to a kind of flaxen fiber, particularly relates to the fine design side of a kind of Herba Apocyni veneti degummed ramie Method.
Background technology
Herba Apocyni veneti, has another name called wild flax, Herba Euphorbiae Helioscopiae fiber crops, red building, apocynum cannabinum etc., is a kind of perennial root herbaceous plant, belongs to Apocynaceae, is widely distributed in the northern area of China, and the integrated distribution Tarimhe River in Xinjiang and Kongquehe are littoral, because of its Xinjiang is spreaded out Plain growth and is most contained and gain the name.Apocynum fibre has many excellent characteristics, soft and good luster, has silk Gloss, the very light of fiber crops, cotton softness, the malleability of floss, and have pharmacological action, be once described as " wild by crudefiber crop expert Feng Yunhe etc. The king of fiber ", therefore it is acknowledged as preferable textile fabric.
Apocynum fibre is a kind of phloem fiber, and it is positioned at the phloem tissue on Herba Apocyni veneti plant stem, in fibre bundle Shape, individuals fibers individualism.Herba Apocyni veneti ultimate fibre is to have in the middle part of cell thin thin in thick and two ends in the middle of a kind of closed at both ends Born of the same parents' shape object, cross section is obvious irregular kidney-shaped, and lumen is less, and fiber is longitudinally without reversing, and there are many vertical lines on surface have Horizontal joint exists.Fibre fineness is about 3~4dtex, and a length of 20~25mm, fiber width is 10~50 μm.
The chemical composition of Herba Apocyni veneti bast and other bast-fibre have certain difference.Herba Apocyni veneti bast hemicellulose level 16.31%, content of lignin 12.09%, it is above Boehmeria Caulis et Folium Lini Fructus Cannabis, especially content of lignin apparently higher than other fiber crops Class, and content of cellulose only 45.74% is minimum in all bast-fibres.
Owing to Herba Apocyni veneti bast non-cellulose components is high, up to nearly the 55% of Herba Apocyni veneti bast, especially hemicellulose and Content of lignin is high, exceedes the 28% of Herba Apocyni veneti bast.Therefore, apocynum degumming is increasingly difficult compared with other bast-fibre, tradition Bast-fibre Degumming method be not appropriate for the degumming process of apocynum fibre, it is necessary to combine Herba Apocyni veneti own characteristic and select to take off Gluing method and technique.
In prior art, conventional apocynum fibre Degumming method is main or the chemical method of traditional bast-fibre degumming, Bioanalysis or Physical.Wherein, chemical method is because using a large amount of chemical reagent to cause waste water to be difficult to process, and environmental pollution is serious, de- Hot conditions energy consumption cost needed for glue is high, and chemical Degumming is difficult between Proper Match fibre strength, length and fineness simultaneously Relation, degumming excessively causes a large amount of short flannel and fibre strength low, the most then fiber residual gum content is high, especially lignin residue amount Height, causes fiber thick and stiff, and flexible little, cohesive force is poor, and the limit count of yarn is low, wiriness, and filoplume is more, and prodding and itching feeling is strong, The premium properties of apocynum fibre can not be fully demonstrated, seriously limit the range of application of apocynum fibre.
For bioanalysis, a lot of bioenzyme activities are not enough, be generally difficult to be applied to apocynum fibre internal component complicated, Compact structure part, is especially difficult to remove lignin portion, and therefore bioanalysis exists that degumming quality is unstable, efficiency is low, consumption Duration, high in cost of production problem, major part is required for chemical method to make up the deficiency of its degumming technology.
Physical Degumming method includes ultrasonic Treatment method, microwave treatment method and steam explosion etc., wherein, applies the most general It is steam explosion technology all over be.But, about in the steam explosion processing procedure of research report, vapor (steam) temperature is high, pressure is big, Particularly, generally require repetition exploding technology repeatedly, inevitably, will result in apocynum fibre strength damage and fiber is long Degree loss.
In a word, for the feature that lignin in Herba Apocyni veneti bast raw material and hemicellulose level are high, not to Herba Apocyni veneti In the case of raw material carries out pretreatment, when relying on single chemistry, biological or physics effect degumming, processing conditions is difficult to Controlling, fibre strength and length, fineness relation are difficult to conservative control, processing gained apocynum fibre or thick, hard, rough, or Fiber strength is low, cast tow rate high, has a strong impact on Herba Apocyni veneti product quality.
In order to improve apocynum fibre performance, promote that it effectively utilizes, both at home and abroad to sieve on the basis of tradition Degumming method Cloth flaxen fiber fine techniques has also carried out a few thing, but is the soft treatment of softening and the textile concentrating on fiber mostly, And not solving the problem that becomes more meticulous of fiber itself, simply softening fibre and reduction fibre-fibre friction power, this is obviously to Herba Apocyni veneti Product is lightening and superior has little significance.
The fine design method of the Herba Apocyni veneti degummed ramie of low damage, is an up the key of apocynum fibre value, Represent the developing direction of industry technology.
Summary of the invention
It is an object of the present invention to provide a kind of fine design method of Herba Apocyni veneti degummed ramie, to overcome prior art The apocynum fibre time-consuming long, that chemical drugs usage amount is big, prepared that Degumming method generally exists is short, thick, hard, intensity is inclined The technical problem such as low.
The present invention be employed technical scheme comprise that for achieving the above object, the fine design side of a kind of Herba Apocyni veneti degummed ramie Method, it is characterised in that comprise the following steps:
The first step, the infiltration activation step of Herba Apocyni veneti bast
Herba Apocyni veneti bast is placed in hermetically sealed can, is immersed in the organic amine that mass percent concentration is 40%~60% molten In agent, it is continuously stirred at room temperature 12~20 hours, so that the infiltration activation of Herba Apocyni veneti bast;
Then, by organic amine solvent vent in tank, take out the Herba Apocyni veneti bast through infiltration activation, standby;
Second step, dodges quick-fried activation process step
By the Herba Apocyni veneti bast after infiltration activation, it is placed in steam explosion device, is passed through steam, until steam explosion In device, the pressure of steam reaches 0.8~1.2MPa, and pressurize 1~5 minutes at this pressure;
Then, rapid pressure release is dodged quick-fried, obtains the Herba Apocyni veneti bast of dispersion activation;
3rd step, beats cake dress cage step
By in the Herba Apocyni veneti bast feeding fiber crops cage of gained dispersion activation, pancake making machine is used to buy cake;When feeding fiber crops, fiber crops cage is with 3~5 Rev/min speed do not stop rotate, pancake making machine machinery foot move up and down beat reality beat Herba Apocyni veneti bast;Meanwhile, watering duckbilled from Up to lower drip washing of spraying water in fiber crops cage continuously, drip washing water temperature is 50 DEG C~80 DEG C;
4th step, directional catalyzing oxidation step
Will be after buying cake and processing, the numb cage being loaded with Herba Apocyni veneti bast is integrally placed in glue kettle, opens liquid feed valve, makes In glue kettle, first inject ferrous salt solution to liquid level with high-pressure pump do not have Herba Apocyni veneti bast;
Then, continue to keep high-pressure pump operating, so that ferrous salt solution is forced to follow with outside ferrous salt solution in glue kettle Ring, in keeping glue kettle, ferrous salt solution is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 15~after 30 minutes, Stop high-pressure pump, close liquid feed valve, open liquid valve, after being emptied by the ferrous salt solution in glue kettle, close liquid valve;
Then, open liquid feed valve, use high-pressure pump first to inject activator body lotion in glue kettle and do not had Herba Apocyni veneti to liquid level Bast;Then, continue to keep high-pressure pump operating, so that activator body lotion and external activator body lotion forced circulation in glue kettle, In keeping glue kettle, activator body lotion is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 1~after 2 hours, stops high pressure Pump, close liquid feed valve, open liquid valve, after being emptied by the activator body lotion in glue kettle, close liquid valve;
Above-mentioned activator is H2O2, peracetic acid or carbamide peroxide solution;
5th step, chemical Degumming step
Open liquid feed valve, in glue kettle, pump into alkalescence degumming liquid, do not had a Herba Apocyni veneti bast to liquid level, heated and boiled, and Continuously cooking 0.5~2 hours under fluidized state;
Then, empty degumming liquid, inject sulphuric acid body lotion or hydrochloric acid body lotion and Herba Apocyni veneti bast is washed to pH value≤7;Make again With clear water rinsed clean repeatedly, obtain apocynum fibre semi-finished product;
6th step, post-processing step
By obtained apocynum fibre semi-finished product successively through being dehydrated, oil, drying, obtain Herba Apocyni veneti degummed ramie finished product.
Be preferably, above-mentioned organic amine solvent be the one in ethylenediamine, dimethylformamide or dimethyl acetylamide or Several.
Further preferably, above-mentioned ferrous salt solution is FeSO4Solution, FeCl2Solution or (NH4)Fe(SO4)2Solution quality hundred Proportion by subtraction concentration is 0.03%~1%.
Further preferably, the mass percent concentration 0.5%~2.5% of above-mentioned activator body lotion, pH value is 3~5, temperature It it is 30 DEG C~50 DEG C;Bath raio is 1 10.
Further preferably, above-mentioned alkalescence degumming liquid be mass percent concentration be the sodium hydroxide solution of 0.1%~1%;
The mass percent concentration of described sulphuric acid body lotion or hydrochloric acid body lotion is 0.1%, and bath raio is 1 20.
Further preferably, the fine design method of above-mentioned Herba Apocyni veneti degummed ramie, it is characterised in that obtained spreads out The fineness of flaxen fiber finished product is 3.3~4.5dtex, and residual gum content is 3.68%~5.22%, and fibre strength is 3.9~7.6cN/ Dtex, the average length of fiber is more than 35mm.
What technique scheme was directly brought has the technical effect that, degumming effect good (residual gum content is 3.68%~5.22%), Obtained apocynum fibre finish fineness thin (being 3.3~4.5dtex), fibre strength index is good (is 3.9~7.6cN/ Dtex), fabric (average length is more than 35mm) of fine quality;
The fine design method of the Herba Apocyni veneti degummed ramie of technique scheme, in whole production process, chemical cost Measuring little, environmental protection pressure to alleviate, technique controlling difficulty is greatly reduced;Utility consumption is little, production efficiency is high for water power vapour etc., life Produce low cost.
For being more fully understood that the technical characterstic of the present invention, show labor and be described as follows:
In technique scheme, Herba Apocyni veneti bast raw material is placed in organic amine solvent, and impregnates under vibration, obtain Sufficient activation processing, raw material becomes fluffy, soft (this is because under the effect of organic amine, in Herba Apocyni veneti bast raw material Hydrogen bond is destroyed, and the colloid such as lignin, hemicellulose, pectin and colloid and colloid weaken with the combination of cellulose, and structure becomes Loose, the amorphous region of cellulose increased and by swollen simultaneously), simultaneously through the activation processing of organic amine, it is possible to decrease final The rigidity of degummed ramie goods, promote its flexibility, can textile processibility and comfort;
Meanwhile, while the short texture that Herba Apocyni veneti bast raw material becomes under the effect of organic amine solvent, after being conducive to Steam and the entrance of aqueous water during continuous steam explosion, strengthen the quick-fried effect of follow-up sudden strain of a muscle.
In technique scheme, will carry out at steam explosion activation through the Herba Apocyni veneti bast of organic amine infiltration activation processing Reason, in the process, the steam of high-temperature high-pressure state and aqueous water act on Herba Apocyni veneti raw material, fill raw material further Divide swelling;Then, under the effect of moment pressure release, make Herba Apocyni veneti bast loosen or disperse, it is achieved the steam of Herba Apocyni veneti bast dodges Quick-fried activation processing.
In technique scheme, during buying cake, use limit to beat cake, the method for limit hot water spray, live to through organic amine infiltration Change processes and dodges the Herba Apocyni veneti bast of quick-fried activation processing and carries out buying cake, and the colloid in Herba Apocyni veneti bast can be made to make in the immersion of warm water With lower further softening, and remove in the effect lower part of mechanical force;Especially, beat during cake due to mechanical external force effect and Warm water process effect, can effectively remove the part Herba Apocyni veneti bast top layer sclerderm that subsequent handling is difficult to remove, and then can be significantly Reduce following process and process intensity, and the consumption of chemical reagent.
It is important to note that in technique scheme, in directional catalyzing oxidizing process, infiltrated activation processing and Loosen after dodging quick-fried activation or the hemicellulose on scattered Herba Apocyni veneti bast surface and lignin under the effect of oxy radical and More Fe is adsorbed under the effect of the nitrogen-containing group of the organic amine brought in organic amine infiltration activation process2+
After adding activator, it is adsorbed with Fe2+Hemicellulose and lignin take the lead in oxidized degraded, the oxidized degraded of part Directly dissolve removal for small organic molecule, part is oxidized to the material that subsequent chemistry degumming is more easy to remove.
In directional catalyzing oxidation step, adsorb Fe2+Herba Apocyni veneti bast, without washing, be i.e. placed directly within containing activator Solution in, it is therefore an objective to protection Fe2+Directional catalyzing activator decomposes, and then oxidative lignin and hemicellulose, strengthens catalysis oxygen Change effect.
Wherein, organic amine infiltration activation, steam explosion activation and Fe are used2+Ion and hydrogen peroxide (or peracetic acid or Carbamide peroxide solution) soak Herba Apocyni veneti bast is oriented one of the key problem in technology point that catalytic oxidation treatment is the present invention, Final apocynum fibre treatment effect is served the most crucial effect.Reason is as follows:
At Herba Apocyni veneti phloem, apocynum fibre cellulose fiber is made in the bonding of the colloids such as pectin, hemicellulose and lignin With lower bunchy (technique) fiber, wherein ultimate fibre a length of 20~25mm, diameter is then 10~50 μm, colloid (pectin, half fiber Element, lignin etc.) rely on hydrogen bond, covalent bond, van der Waals interaction to be connected with each other with cellulose, these gum dispersion are in the fibre Between or be enclosed in outside fiber, define densification Network Three-dimensional space structure so that cellulosic sections be difficult to dispersion.Traditional is de- Gluing method is all made by the effect of chemical reagent or enzyme, the most successively the colloid in bundle fiber is stripped down, and causes Making degumming degree inside and outside raw material inconsistent, outer layer degumming degree is better than internal layer, causes end article quality to decline, simultaneously this process Reaction condition is wayward, if degumming effect is violent, fiber can be caused to shorten, lose weaving use value;If degumming effect Bad, residual gum content is higher, and fiber will be caused thick, hard, rough, is unfavorable for that follow-up textile process operation uses equally.
Therefore, to change the degumming mode the most successively peeling off colloid, with condition Proper Match sieve of milder Relation between cloth fiber crops process of fiber intensity, fineness, length, needs the orientation that raw material carries out part non-cellulosic material to remove.
And the organic amine infiltration activating pretreatment of technique scheme, it is not destroy apocynum fibre bulk composition fiber In the case of the element degree of polymerization, destroy that the component molecules such as lignin, hemicellulose in raw material is interior and intermolecular and lignin, half fibre Hydrogen bond between dimension element and cellulosic molecule, weakens the adhesion of colloid and colloid and colloid and cellulose, increases raw material simultaneously Swollen degree, the infiltration of partial removal hemicellulose and lignin, beneficially degumming reagent is also had an effect further.Meanwhile, Using organic amine as activating reagent, it is also possible on the one hand increase its water solublity with lignin effect, on the other hand possess brilliant work that disappear With, material crystal degree can be reduced, increase amorphous region area, improve raw material hydrophilic, therefore, be more beneficial for reducing further The difficulty of follow-up degumming.
What is more important, under the effect of organic amine, in Herba Apocyni veneti bast raw material, the composition such as lignin, hemicellulose divides The destruction of hydrogen bond between son interior and intermolecular and lignin, hemicellulose and cellulosic molecule, colloid and colloid and colloid and Weakening of cellulose adhesion, the increase of raw material swollen degree, make that the tough skin structure of Herba Apocyni veneti becomes is loose, and then makes raw material compare table While area increases, owing to the colloid such as hemicellulose and lignin is wrapped in fibrous outer, it is thus in the half of raw material surface Cellulose and content of lignin increase, and make more group containing O be exposed to raw material surface, power containing O at hemicellulose and lignin Under the effect of subbase group, can the more Fe of active adsorption2+Ion, enhances Herba Apocyni veneti bast raw material Fe2+The activity of ionic adsorption, Simultaneously in organic amine infiltration activation process, Herba Apocyni veneti bast raw material can bring organic amine material into, in organic amine containing nitrilo Group also can strengthen Herba Apocyni veneti bast raw material Fe2+The activity of ionic adsorption, Fe in follow-up orientation activation process2+The suction of ion Attached, and then the carrying out of follow-up directional catalyzing oxidation.
It addition, the steam explosion activation processing of technique scheme, because steam explosion process intensity is low, so, can be not In the case of destroying apocynum fibre bulk composition cellulosic degree of polymerization, destroy lignin, hemicellulose etc. in raw material further Component molecules is interior and intermolecular and hydrogen bond between lignin, hemicellulose and cellulosic molecule, weaken colloid and colloid and The adhesion of colloid and cellulose, increases the swollen degree of raw material simultaneously, and partial removal hemicellulose and lignin are follow-up The infiltration of chemical reagent is also had an effect further.
Meanwhile, in the steam explosion activated process of technique scheme, high temperature, the steam of high pressure conditions and liquid Water acts on the Herba Apocyni veneti bast raw material through organic amine infiltration activation, and raw material carries out abundant swollen, moment pressure release subsequently Cheng Zhong, under the synergy of class mechanical disintegration effect, hydrogen bond destruction and structural rearrangement, hemicellulose and hemicellulose Between, connection between hemicellulose and lignin, between hemicellulose and cellulose, between lignin and cellulose fracture or Weakening, raw material is loosened or is disperseed, and makes Herba Apocyni veneti bast raw material specific surface area increase, can strengthen follow-up Fe2+The absorption of ion. Meanwhile, during steam explosion, under the effect of class acidic hydrolysis and thermal degradation, part hemicellulose degradation can be made to go Remove, reduce following process and process intensity and chemical levels.
What is more important, in steam explosion activation process, due to class mechanical disintegration effect, hydrogen bond destruction and The synergy of structural rearrangement, cause between hemicellulose and hemicellulose, between hemicellulose and lignin, hemicellulose with Connection between cellulose, between lignin and cellulose is ruptured or weakens, and makes Herba Apocyni veneti raw material be loosened or disperse, makes former While material specific surface area increases, owing to the colloid such as hemicellulose and lignin is wrapped in fibrous outer, it is thus in stock chart The hemicellulose in face and content of lignin increase, and make more group containing O be exposed to raw material surface, contain at hemicellulose and lignin Under the effect of O electron-donating group, can the more Fe of active adsorption2+Ion, enhances Herba Apocyni veneti bast raw material Fe2+Ionic adsorption Activity, Fe in follow-up orientation activation process2+The absorption of ion, and then the carrying out of follow-up directional catalyzing oxidation.
It addition, in dodging quick-fried activation process, the steam of high-temperature high-pressure state and aqueous water, can be well to being difficult to remove Herba Apocyni veneti bast crust carry out effective swollen, in moment pressure leak process subsequently under class mechanical disintegration effect, by itself and sieve The cloth tough endo-endothelial layer of fiber crops separates and removes, and reduces the oxidation of follow-up directional catalyzing and the difficulty of soda boiling process and intensity, reduces follow-upization Learn the usage amount of reagent.
Meanwhile, in dodging quick-fried activation process, in class mechanical disintegration effect, hydrogen bond destruction and the associating of structural rearrangement Under effect, Herba Apocyni veneti bast raw material has obtained effectively loosening or disperseing, takes off with chemical Degumming method and the biology of prior art Gluing method is compared, can save after soda boiling degumming copy fiber crops step, reduce energy consumption and water consumption.
In directional catalyzing oxidizing process, through organic amine infiltration activation processing and the Herba Apocyni veneti raw material of the quick-fried activation processing of sudden strain of a muscle, Due to increasing and the introducing of nitrogen-containing group, at FeSO of hemicellulose and lignin Surface oxygen-containing groups4、FeCl2Or (NH4) Fe(SO4)2Under the immersion of solution, Fe is adsorbed on Herba Apocyni veneti raw material surface in a large number2+, then in hydrogen peroxide or peracetic acid or peroxidating During urea liquid processes, hemicellulose and the Fe of lignin absorption2+Directly add at hemicellulose and lignin surface catalysis H2O2Or the H that peracetic acid or the hydrolysis of carbamide peroxide solution generate2O2Decompose, in acid condition, Fe2+Catalysis H2O2Decompose and produce The HO that raw oxidability is extremely strong, the HO extremely strong due to the oxidability of generation are predominantly located at hemicellulose and lignin table Face, therefore can be degraded to water soluble small organic molecule by part hemicellulose and be dissolved in the water;Simultaneously because HO oxidability is extremely strong, can be raw by complicated for structure and be difficult to the lignin side chain C-C bond fission removed or ring-opening reaction occurs Subsequent chemistry degumming is become to be more easy to the structure removed, it is easy to follow-up degumming is removed.HO Oxidation radius is the least simultaneously, and due to Cellulose is wrapped in hemicellulose and lignin, and therefore the Oxidation of HO is difficult to make cellulose oxidation degrade.
During chemical Degumming, high temperature alkaline solution can hydrolyze removal and remain most non-cellulosic material, especially may be used Make oxidized rear side chain C-C bond fission or the lignin generation hydrolysis of ring-opening reaction occur and removes so that fiber enters one Step dispersion, cellulose disappears brilliant effect under alkali liquor simultaneously, reduces degree of crystallinity, the hydrophilic of raising fiber, softening fibre.
Herba Apocyni veneti bast raw material in technique scheme, after infiltration activating pretreatment, it is not necessary to washing, the most directly enters Row steam explosion pretreatment.Main cause, one is in steam explosion preprocessing process, and the organic amine having neither part nor lot in priming reaction enters Herba Apocyni veneti bast is activated by one step, and two is to effectively protect the organic amine activation effect to Herba Apocyni veneti bast raw material.
In technique scheme, break the Herba Apocyni veneti bast raw material after cake, it is not necessary to washing, be i.e. directly injected into ferrous salt solution and enter Row processes, and main cause is, the residue organic amine reagent removed the most completely during buying cake, and former with apocynum fibre There is the organic amine reagent of chemical reaction in material, under the left and right of the N element that can contain at organic amine self, adsorbs more Fe2+, increase Strong catalytic oxidation effect.
In technique scheme, the Herba Apocyni veneti bast raw material that why will aoxidize through directional catalyzing, it is not necessary to washing, i.e. exist After emptying reactant liquor, it is pumped directly into alkali liquor and carries out degumming process, it is therefore intended that, one is, wherein remaining undecomposed activator can To increase the degumming effect in soda boiling scouring processes and bleaching effect, two are, remaining Fe2+Degumming liquid can carry out coagulation take off Color, alleviates subsequent wastewater treatment difficulty.
Certainly, correspondingly, the pre-acid treatment with prior art, pre-alkali process, pre-urine oxygen processes chemical Degumming method contrast, Before chemical Degumming, eliminate a water-washing step, reduce water consumption.
It addition, compared with existing biology, chemical Degumming technology, this technology is due to remaining Fe2+Ion is in chemical Degumming mistake Journey has coagulation decoloration effect, the coloring matter in effluent part can be taken off.Therefore, to produced during subsequent production Waste water decoloring intractability reduces accordingly.
Meanwhile, with the chemical Degumming method ratio of prior art, technique scheme needs not move through the length of a large amount of chemical reagent Time steaming and decocting, by Fe under steam explosion and acid condition2+The selective paraffin oxidation degraded of the HO that ionic catalysis activator produces is made There is efficiency height with carrying out apocynum fibre degumming, pollute the significant advantages such as little.
In technique scheme, pickling then in order to neutralize the alkaline reagent of chemical Degumming, prevents alkali from cellulose is entered one Step degraded;Oil to improve the apparent condition of fiber, increase laxity and the softness of fiber, it is simple to follow-up spinning.
In a word, just because of the combination of above-mentioned series technique means so that when apocynum fibre crude product alkaline boiling, The steaming and decocting of relatively prior art processes, and is all greatly decreased or saves in terms of chemical levels, steaming and decocting required time, and this is for having Effect alleviates the damage to fibrous physics index of the alkaline scouring process, reduces waste water intractability, alleviates environmental protection pressure, raising production effect Rate, reduces production cost and is respectively provided with obvious positive effect.
Supplementary notes: in technique scheme, the apocynum fibre after alkaline scouring processes, colloid remaining in fiber And pigment, removed further, thus reached ideal flax fiber separation index and whiteness index.
In sum, the present invention, relative to prior art, has the advantages that
1, degumming effect good (residual gum content is 3.68%~5.22%), the Herba Apocyni veneti degummed ramie finish fineness obtained is thin (being 3.3~4.5dtex), fibre strength index good (being 3.9~7.6cN/dtex), (average length is big for average fiber length length In 35mm), good spinnability;
2, chemical cost amount is little, environmental protection pressure alleviates, and technique controlling difficulty is greatly reduced;
3, utility consumption is little, production efficiency is high, production cost is greatly reduced for water, electricity, vapour etc..
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail.
Embodiment 1
The Herba Apocyni veneti bast places of origin of raw materials: Xinjiang
Processing method is as follows:
Herba Apocyni veneti bast is placed in hermetically sealed can, is immersed in the ethylenediamine that mass percent concentration is 40%, in room temperature Under continuously stirred 12 hours so that Herba Apocyni veneti bast infiltration activation;
Then, ethylenediamine in tank is vented, takes out the Herba Apocyni veneti bast through infiltration activation.
Being directly placed in steam explosion device by Herba Apocyni veneti raw material after ethylenediamine infiltration activation, heating makes steam explosion fill Putting interior water vapour pressure is 0.8MPa, keeps this pressure 1 minute;Then valve, rapid pressure release are opened;
Collect from steam explosion equipment ejection apocynum fibre, then carry out beat cake, will beat cake gained Herba Apocyni veneti tough Skin and fiber crops cage are together placed in glue kettle, pump into the FeSO that mass percent concentration is 0.05%4Solution, to not having Herba Apocyni veneti tough Skin, at room temperature, uses high-pressure pump to make FeSO4Solution inner-outer circulation 15 minutes, empties FeSO4After solution, pump into mass percent Concentration is the hydrogen peroxide solution of 0.5%, after 30 DEG C of circular treatment 1 hour, emptying hydrogen peroxide solution, pumps into mass percent dense Degree is the sodium hydroxide solution of 0.1%, and boiling boils 1 hour.
Then, the fiber after steaming and decocting is at room temperature carried out pickling, pickle be mass percent concentration be the sulfur of 0.1% Acid or solution (acid cleaning process, selection bath raio is 1:20), pickling time is 5 minutes.
It is neutral by fiber washing to pH value, finally, successively after being dehydrated, oil, drying, obtains fine Herba Apocyni veneti fine Dimension.
Examination and test of products testing result:
Obtained Herba Apocyni veneti degummed ramie residual gum content is 5.22%, and average fiber length is more than 35mm, and fibre strength is 7.6cN/dtex, fibre fineness is 4.5dtex.
Embodiment 2
The Herba Apocyni veneti bast places of origin of raw materials: Xinjiang
Processing method is as follows:
Herba Apocyni veneti bast is placed in hermetically sealed can, is immersed in the solvent dimethylformamide that mass percent concentration is 60% In, it is continuously stirred at room temperature 20 hours, so that the infiltration activation of Herba Apocyni veneti bast;
Then, dimethylformamide in tank is vented, takes out the Herba Apocyni veneti bast through infiltration activation.
By dimethylformamide infiltration activation
After Herba Apocyni veneti raw material be directly placed in steam explosion device, heating makes the water vapour pressure in steam explosion device For 1.2MPa, keep this pressure 5 minutes;Then valve, rapid pressure release are opened;
Collect from steam explosion equipment ejection apocynum fibre, then carry out beat cake, will beat cake gained Herba Apocyni veneti tough Skin and fiber crops cage are together placed in glue kettle, pump into the FeCl that mass percent concentration is 0.1%2Solution, to not having Herba Apocyni veneti tough Skin, at room temperature, uses high-pressure pump to make FeCl2Solution inner-outer circulation 30 minutes, empties FeCl2After solution, pump into mass percent Concentration is the peracetic acid soln of 2.5%, after 50 DEG C of circular treatment 1 hour, emptying peracetic acid soln, pumps into percent mass Specific concentration is the sodium hydroxide solution of 0.1%, and boiling boils 0.5 hour.
Then, the fiber after steaming and decocting is at room temperature carried out pickling, pickle be mass percent concentration be the salt of 0.1% Acid solution (acid cleaning process, selection bath raio is 1:20), pickling time is 5 minutes.
It is neutral by fiber washing to pH value, finally, successively after being dehydrated, oil, drying, obtains fine Herba Apocyni veneti fine Dimension.
Examination and test of products testing result:
Obtained Herba Apocyni veneti degummed ramie residual gum content is 3.68%, and average fiber length is more than 35mm, and fibre strength is 3.9cN/dtex, fibre fineness is 3.3dtex.
Embodiment 3
The Herba Apocyni veneti bast places of origin of raw materials: Xinjiang
Processing method: except FeSO4Solution quality percent concentration is 1%, the time of alkalescence degumming liquid continuously cooking is 2 little Time, use carbamide peroxide solution substitute hydrogen peroxide, use dimethyl acetylamide replace ethylenediamine, the matter of carbamide peroxide solution Outside amount percent concentration is 1.5%;
Remaining, all with embodiment 1.
Examination and test of products testing result:
Obtained Herba Apocyni veneti degummed ramie residual gum content is 4.62%, and average fiber length is more than 35mm, and fibre strength is 6.2cN/dtex, fibre fineness is 4.0dtex.
It should be noted that organic amine solvent used in the present invention can also is that ethylenediamine, dimethylformamide or Mixing or the mixture of three two-by-two of dimethyl acetylamide.

Claims (6)

1. the fine design method of a Herba Apocyni veneti degummed ramie, it is characterised in that comprise the following steps:
The first step, the infiltration activation step of Herba Apocyni veneti bast
Herba Apocyni veneti bast is placed in hermetically sealed can, is immersed in the organic amine solvent that mass percent concentration is 40%~60% In, it is continuously stirred at room temperature 12~20 hours, so that the infiltration activation of Herba Apocyni veneti bast;
Then, by organic amine solvent vent in tank, take out the Herba Apocyni veneti bast through infiltration activation, standby;
Second step, dodges quick-fried activation process step
By the Herba Apocyni veneti bast after infiltration activation, it is placed in steam explosion device, is passed through steam, until steam explosion device The pressure of interior steam reaches 0.8~1.2MPa, and pressurize 1~5 minutes at this pressure;
Then, rapid pressure release is dodged quick-fried, obtains the Herba Apocyni veneti bast of dispersion activation;
3rd step, beats cake dress cage step
By in the Herba Apocyni veneti bast feeding fiber crops cage of gained dispersion activation, pancake making machine is used to buy cake;Feed fiber crops time, fiber crops cage with 3~5 turns/ Minute speed do not stop rotate, pancake making machine machinery foot move up and down beat reality beat Herba Apocyni veneti bast;Meanwhile, watering duckbilled is from up to Lower drip washing of spraying water in fiber crops cage continuously, drip washing water temperature is 50 DEG C~80 DEG C;
4th step, directional catalyzing oxidation step
Will be after buying cake and processing, the numb cage being loaded with Herba Apocyni veneti bast is integrally placed in glue kettle, opens liquid feed valve, uses height Press pump first injects ferrous salt solution to liquid level in glue kettle and did not had Herba Apocyni veneti bast;
Then, continue to keep high-pressure pump operating, so that ferrous salt solution and outside ferrous salt solution forced circulation in glue kettle, protect In holding glue kettle, ferrous salt solution is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 15~after 30 minutes, stops high pressure Pump, close liquid feed valve, open liquid valve, after being emptied by the ferrous salt solution in glue kettle, close liquid valve;
Then, open liquid feed valve, use high-pressure pump first to inject activator body lotion to liquid level in glue kettle and do not had Herba Apocyni veneti bast; Then, continue to keep high-pressure pump operating, so that activator body lotion and external activator body lotion forced circulation in glue kettle, keep de- In glue tank, activator body lotion is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 1~after 2 hours, stops high-pressure pump, pass Close liquid feed valve, open liquid valve, after being emptied by the activator body lotion in glue kettle, close liquid valve;
Above-mentioned activator is H2O2, peracetic acid or carbamide peroxide solution;
5th step, chemical Degumming step
Open liquid feed valve, in glue kettle, pump into alkalescence degumming liquid, do not had Herba Apocyni veneti bast, heated and boiled to liquid level, and boiling Rise under state continuously cooking 0.5~2 hours;
Then, empty degumming liquid, inject sulphuric acid body lotion or hydrochloric acid body lotion and Herba Apocyni veneti bast is washed to pH value≤7;Re-use clear Water rinsed clean repeatedly, obtains apocynum fibre semi-finished product;
6th step, post-processing step
By obtained apocynum fibre semi-finished product successively through being dehydrated, oil, drying, obtain Herba Apocyni veneti degummed ramie finished product.
The fine design method of apocynum fibre the most according to claim 1, it is characterised in that described organic amine is molten Agent is one or more in ethylenediamine, dimethylformamide or dimethyl acetylamide.
The fine design method of Herba Apocyni veneti degummed ramie the most according to claim 1, it is characterised in that described ferrous salt is molten Liquid is FeSO4Solution, FeCl2Solution or (NH4)Fe(SO4)2, mass percent concentration is 0.03%~1%.
The fine design method of Herba Apocyni veneti degummed ramie the most according to claim 1, it is characterised in that described activator is bathed The mass percent concentration of liquid is 0.5%~2.5%, and pH value is 3~5, and temperature is 30 DEG C~50 DEG C;Bath raio is 1 10.
5. according to the fine design method of the arbitrary described Herba Apocyni veneti degummed ramie of claim 1-4, it is characterised in that described alkali Property degumming liquid be mass percent concentration be the sodium hydroxide solution of 0.1%~1%;
The mass percent concentration of described sulphuric acid body lotion or hydrochloric acid body lotion is 0.1%, and bath raio is 1 20.
6. according to the fine design method of the arbitrary described Herba Apocyni veneti degummed ramie of claim 1-4, it is characterised in that obtained The fineness 3.3~4.5dtex of Herba Apocyni veneti degummed ramie finished product, residual gum content is 3.68%~5.22%, fibre strength be 3.9~ 7.6cN/dtex, the average length of fiber is more than 35mm.
CN201610953766.0A 2016-10-27 2016-10-27 A kind of fine design method of bluish dogbane degummed ramie Active CN106319642B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610953766.0A CN106319642B (en) 2016-10-27 2016-10-27 A kind of fine design method of bluish dogbane degummed ramie

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610953766.0A CN106319642B (en) 2016-10-27 2016-10-27 A kind of fine design method of bluish dogbane degummed ramie

Publications (2)

Publication Number Publication Date
CN106319642A true CN106319642A (en) 2017-01-11
CN106319642B CN106319642B (en) 2018-08-24

Family

ID=57819065

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610953766.0A Active CN106319642B (en) 2016-10-27 2016-10-27 A kind of fine design method of bluish dogbane degummed ramie

Country Status (1)

Country Link
CN (1) CN106319642B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108532000A (en) * 2018-04-17 2018-09-14 中国农业科学院麻类研究所 A kind of Degumming method of bluish dogbane bast
CN109487539A (en) * 2018-09-30 2019-03-19 杭州创屹机电科技有限公司 A kind of processing method improving linen-cotton feel
CN111607898A (en) * 2020-04-26 2020-09-01 马建伟 Production process of high-performance composite material based on China hemp fibers

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040191888A1 (en) * 2001-07-10 2004-09-30 Clarke Adrian Francis K. Degumming of bast fibres
CN103255484A (en) * 2013-05-31 2013-08-21 新疆大学 Refined and degummed cotton stalk bark fiber and preparation method thereof
KR20140062642A (en) * 2012-11-14 2014-05-26 이경종 Degumming method of bast fiber
CN105256384A (en) * 2015-10-20 2016-01-20 东华大学 Method for oxidation degumming of ramie under weak acid condition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040191888A1 (en) * 2001-07-10 2004-09-30 Clarke Adrian Francis K. Degumming of bast fibres
KR20140062642A (en) * 2012-11-14 2014-05-26 이경종 Degumming method of bast fiber
CN103255484A (en) * 2013-05-31 2013-08-21 新疆大学 Refined and degummed cotton stalk bark fiber and preparation method thereof
CN105256384A (en) * 2015-10-20 2016-01-20 东华大学 Method for oxidation degumming of ramie under weak acid condition

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
唐志翔: ""用于废水处理的新颖纤维素类吸附剂"", 《染整技术》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108532000A (en) * 2018-04-17 2018-09-14 中国农业科学院麻类研究所 A kind of Degumming method of bluish dogbane bast
CN108532000B (en) * 2018-04-17 2020-07-10 中国农业科学院麻类研究所 Degumming method of apocynum venetum bast
CN109487539A (en) * 2018-09-30 2019-03-19 杭州创屹机电科技有限公司 A kind of processing method improving linen-cotton feel
CN111607898A (en) * 2020-04-26 2020-09-01 马建伟 Production process of high-performance composite material based on China hemp fibers

Also Published As

Publication number Publication date
CN106319642B (en) 2018-08-24

Similar Documents

Publication Publication Date Title
CN106435760B (en) A kind of fine design method of apocynum fibre
CN106567138B (en) A kind of fine design method of hemp
CN101638811A (en) Degumming technology of mulberry bark
CN106435757B (en) A kind of fine design method of flax fiber
CN106400128B (en) A kind of fine design method of ramee
CN106319642A (en) Refining processing method for apocynum venetum fiber
CN105256626B (en) A kind of mulberry skin chemi-mechanical pulp and preparation method thereof and purposes
CN101298701A (en) Cotton stalk pholeom fiber and degum processing method thereof
CN104032380B (en) A kind of preparation method of mulberry fibre
CN104178819B (en) The freezing shock heating lignoenzyme auxiliary degumming process of a kind of china-hemp fibers
CN100352993C (en) Bleaching method of fenther fabric
CN106400127B (en) A kind of fine design method of sisal fiber
CN106435756B (en) A kind of fining production method of bluish dogbane degummed ramie
CN106567140B (en) A kind of fining production method of the keen-witted and capable flaxen fiber of bluish dogbane
CN110894696A (en) Method for bleaching bamboo pulp
WO2005064076A1 (en) Closed cycle zero discharge oxidizing pulping process
CN106801355B (en) A kind of bamboo wood autoclaving technique reducing bamboo Kun losses
CN103469535A (en) Low-temperature pre-treatment technology of cotton fabric
CN101105005A (en) Method for increasing deep color stability of hemp cloth
CN106435758B (en) A kind of fine design method of bastose
CN106567139B (en) A kind of production method of bluish dogbane degummed ramie
CN103484949A (en) Degumming process for mulberry fibers
CN101411885A (en) Novel technique for dewatering and rinsing medical dressing by one-bath method
CN106567136B (en) A kind of fining production method of apocynum fibre
CN102797162A (en) Pretreatment method for cotton fabric with enzyme and hydrogen peroxide in one bath

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant