CN106319642B - A kind of fine design method of bluish dogbane degummed ramie - Google Patents

A kind of fine design method of bluish dogbane degummed ramie Download PDF

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CN106319642B
CN106319642B CN201610953766.0A CN201610953766A CN106319642B CN 106319642 B CN106319642 B CN 106319642B CN 201610953766 A CN201610953766 A CN 201610953766A CN 106319642 B CN106319642 B CN 106319642B
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bluish dogbane
bast
liquid
activation
degumming
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CN106319642A (en
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张元明
韩光亭
徐颖
徐维敬
李洋
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Qingdao University
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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

Abstract

The invention discloses a kind of fine design method of bluish dogbane degummed ramie, including bluish dogbane bast infiltration activation, steam explosion activation process, beat cake dress cage, directional catalyzing oxidation, chemical Degumming and post-processing step;After it is by organic amine infiltration activation and steam explosion activation process, catalytic oxidation treatment is oriented to lignin and hemicellulose using ferrous salt solution and activator;And the combination by infiltrating the series techniques means such as activation, steam explosion and directional catalyzing oxidation, so that the production method of the present invention, the features such as indexs such as, the bluish dogbane degummed ramie 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, 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 bluish dogbane degummed ramie
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 bluish dogbane degummed ramie 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 fine design method of the bluish dogbane degummed ramie of low damage is the key that promote apocynum fibre utility value, Represent the developing direction of industry technology.
Invention content
It is an object of the present invention to provide a kind of fine design methods of bluish dogbane degummed ramie, to overcome the prior art The apocynum fibre that time-consuming for Degumming method generally existing, chemicals usage amount is big, prepared is short, thick, hard, intensity is inclined Low technical problem.
Present invention technical solution used for the above purpose is a kind of fine design side of bluish dogbane degummed ramie 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 hermetically sealed can, it is molten to be immersed in the organic amine that mass percent concentration is 40%~60% It in agent, is continuously stirred at room temperature 12~20 hours, so that the infiltration activation of bluish dogbane bast;
Then, by organic amine solvent vent in tank, the bluish dogbane bast by infiltration activation is taken out, it is spare;
Second step dodges quick-fried activation process step
It by the bluish dogbane bast after infiltration activates, is placed in steam explosion device, is passed through steam, until steam explosion The pressure of vapor reaches 0.8~1.2MPa, and pressurize 1~5 minute at this pressure in device;
Then, rapid pressure release is dodged quick-fried, obtains the bluish dogbane bast of dispersion activation;
Third walks, and beats cake dress cage step
By in the numb cage of bluish dogbane bast feeding of gained dispersion activation, cake is beaten using pancake making machine;When feeding fiber crops, 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;
4th step, 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, Keep glue kettle in activator bath foam always with swiftly flowing state constant impingement bluish dogbane bast 1~2 hour after, stop high pressure 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;
5th 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;
6th step, post-processing step
By obtained apocynum fibre semi-finished product successively through being dehydrated, oiling, dry to get bluish dogbane degummed ramie 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, FeCl2Solution or (NH4)Fe(SO4)2Solution quality hundred It is 0.03%~1% to divide specific concentration.
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 bath foam or hydrochloric acid bath foam is 0.1%, and bath raio is 1 ︰ 20.
Further preferably, the fine design method of above-mentioned bluish dogbane degummed ramie, which is characterized 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/ 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 3.3~4.5dtex), fibre strength index are good (for 3.9~7.6cN/ Dtex), fabric is (average length is more than 35mm) of fine quality;
The fine design method of the bluish dogbane degummed ramie of above-mentioned technical proposal, in entire production process, chemical cost It measures small, environmental protection pressure to mitigate, technique controlling difficulty is greatly reduced;The utility consumptions such as water power vapour are small, production efficiency is high, raw It produces 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;
Meanwhile bluish dogbane bast raw material become under the action of organic amine solvent short texture while, after being conducive to Quick-fried effect is subsequently dodged in the entrance of vapor and liquid water, enhancing during continuous steam explosion.
In above-mentioned technical proposal, the bluish dogbane bast that activation process is infiltrated by organic amine is carried out at steam explosion activation Reason, in the process, the vapor and liquid water of high-temperature high-pressure state act on bluish dogbane raw material, are further filled to raw material Divide swelling;Then, under the action of moment pressure release, bluish dogbane bast is made to loosen or disperse, realizes that the steam of bluish dogbane bast dodges Quick-fried activation process.
In above-mentioned technical proposal, beat during cake using while beat cake, while hot water spray method, to through organic amine infiltration work Change processing and the bluish dogbane bast for dodging quick-fried activation process carry out buying cake, and the colloid in bluish dogbane bast can be made to make in the immersion of warm water With lower further softening, and partly removed under the action of mechanical force;Especially, beat during cake due to mechanical external force effect and Warm water processing acts on, and can effectively remove the part bluish dogbane bast surface layer sclerderm that subsequent handling is difficult to remove, and then can be substantially Reduce the consumption of following process processing intensity and chemical reagent.
It is important to note that in above-mentioned technical proposal, in directional catalyzing oxidation process, infiltrated activation process and The hemicellulose and lignin on the bluish dogbane bast surface loosened or disperseed after dodging quick-fried activation under the action of oxygen-containing group and More Fe are adsorbed under the action of organic amine infiltrates the nitrogen-containing group for the organic amine brought into activation process2+
After activator is added, it is adsorbed with Fe2+Hemicellulose and lignin take the lead in by oxidative degradation, partly by oxidative degradation Removal is directly dissolved for small organic molecule, 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 and hemicellulose, enhancing catalysis oxygen Change effect.
Wherein, using organic amine infiltration activation, steam explosion activation and Fe2+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, Very crucial effect is played to final apocynum fibre treatment 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 of above-mentioned technical proposal infiltrates activating pretreatment, is not destroy apocynum fibre bulk composition fiber In the case of the plain degree of polymerization, destroy that the component molecules such as lignin, hemicellulose in raw material are interior and intermolecular and lignin, half fiber Hydrogen bond between dimension element and cellulosic molecule, reduction colloid and colloid and the binding force of colloid and cellulose, while increasing raw material Swollen degree, partial removal hemicellulose and lignin, conducive to degumming reagent infiltration and further have an effect.Meanwhile Using organic amine as activating reagent, it on the one hand can also increase its water solubility with lignin effect, on the other hand have brilliant make that disappear With can reduce material crystal degree, increase amorphous region area, improve raw material hydrophily and be therefore more advantageous to and further decrease The difficulty of follow-up degumming.
What is more important, under the action of organic amine, the ingredients such as lignin, hemicellulose point in bluish dogbane bast raw material The destruction of hydrogen bond between sub interior and intermolecular and lignin, hemicellulose and cellulosic molecule, colloid and colloid and colloid and The decrease of cellulose binding force, the increase of raw material swollen degree make the tough skin structure of bluish dogbane become loose, and then raw material are made to compare table Area is increased simultaneously as the colloids such as hemicellulose and lignin are wrapped in fibrous outer, therefore half in raw material surface Cellulose and content of lignin increase, and more groups containing O is made to be exposed to raw material surface, power containing O in hemicellulose and lignin Under the action of subbase group, more Fe can be effectively adsorbed2+Ion enhances bluish dogbane bast raw material Fe2+The activity of ionic adsorption, Simultaneously in organic amine infiltrates activation process, organic amine substance can be brought in bluish dogbane bast raw material into, the nitrogenous base in organic amine Group can also enhance bluish dogbane bast raw material Fe2+The activity of ionic adsorption is conducive to Fe in follow-up orientation activation process2+The suction of ion It is attached, and then be conducive to the progress of follow-up directional catalyzing oxidation.
In addition, the steam explosion activation process of above-mentioned technical proposal, because steam explosion processing intensity is low, so, it can be not In the case of destroying apocynum fibre bulk composition cellulosic degree of polymerization, lignin, hemicellulose etc. in raw material are further destroyed Component molecules are interior and hydrogen bond between intermolecular and lignin, hemicellulose and cellulosic molecule, reduction colloid and colloid and The binding force of colloid and cellulose, while increasing the swollen degree of raw material, partial removal hemicellulose and lignin, it is conducive to follow-up The infiltration of chemical reagent is simultaneously further had an effect.
Meanwhile in the steam explosion activation process of above-mentioned technical proposal, high temperature, the vapor of high pressure conditions and liquid Water acts on the bluish dogbane bast raw material through organic amine infiltration activation, and abundant swollen, subsequent moment pressure release are carried out to raw material Cheng Zhong, under the effect of class mechanical disintegration, hydrogen bond destruction and the synergy of structural rearrangement, hemicellulose and hemicellulose Between, the connection fracture between hemicellulose and lignin, between hemicellulose and cellulose, between lignin and cellulose or Weaken, raw material is loosened or disperseed, and so that bluish dogbane bast raw material specific surface area is increased, can enhance follow-up Fe2+The absorption of ion. Meanwhile during steam explosion, under the action of class acidic hydrolysis and thermal degradation, part hemicellulose degradation can be made to go It removes, reduces following process processing 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 fracture between cellulose, between lignin and cellulose or decrease, make bluish dogbane raw material be loosened or be disperseed, make original Material specific surface area is increased simultaneously as the colloids such as hemicellulose and lignin are wrapped in fibrous outer, therefore are in stock chart The hemicellulose and content of lignin in face increase, and so that more groups containing O is exposed to raw material surface, contain in hemicellulose and lignin Under the action of O electron-donating groups, more Fe can be effectively adsorbed2+Ion enhances bluish dogbane bast raw material Fe2+Ionic adsorption Activity is conducive to Fe in follow-up orientation activation process2+The absorption of ion, and then be conducive to the progress of follow-up directional catalyzing oxidation.
In addition, in dodging quick-fried activation process, the vapor and liquid water of high-temperature high-pressure state can be well to being not easy to remove Bluish dogbane bast crust carry out effective swollen, in subsequent moment pressure leak process under the effect of class mechanical disintegration, by itself and sieve The tough endo-endothelial layer of cloth fiber crops is detached and is removed, and is reduced the difficulty and intensity of follow-up directional catalyzing oxidation and soda boiling processing, is reduced follow-upization Learn the usage amount of reagent.
Meanwhile in dodging quick-fried activation process, in the joint of the effect of class mechanical disintegration, hydrogen bond destruction and structural rearrangement Under effect, bluish dogbane bast raw material has obtained effectively loosening or disperseing, de- with the chemical Degumming method and biology of the prior art Gluing method is compared, and can be saved and be copied numb step after soda boiling degumming, reduce energy consumption and water consume.
In directional catalyzing oxidation process, the bluish dogbane raw material through organic amine infiltration activation process and the quick-fried activation process of sudden strain of a muscle, Due to hemicellulose and lignin Surface oxygen-containing groups increase and the introducing of nitrogen-containing group, in FeSO4、FeCl2Or (NH4) Fe(SO4)2Under the immersion of solution, Fe is largely adsorbed on bluish dogbane raw material surface2+, then in hydrogen peroxide or Peracetic acid or peroxidating In urea liquid processing, the Fe of hemicellulose and lignin absorption2+It is directly added in hemicellulose and lignin surface catalysis H2O2Or the H that Peracetic acid or the hydrolysis of carbamide peroxide solution generate2O2It decomposes, in acid condition, Fe2+It is catalyzed H2O2Decompose production The extremely strong HO of raw oxidability, since the extremely strong HO of the oxidability of generation is predominantly located at hemicellulose and lignin table Face, therefore can part hemicellulose be degraded to water soluble small organic molecule and be 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 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, without washing, i.e., directly into Row steam explosion pre-processes.Main cause, first, in steam explosion preprocessing process, have neither part nor lot in the organic amine of priming reaction into One step activates bluish dogbane bast, 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 steam explosion and acid condition2+The selective paraffin oxidation degradation for the HO that ionic catalysis activator generates is made There are the significant advantages such as efficient, pollution is small with apocynum fibre degumming is carried out.
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, degumming effect is good (residual gum content is 3.68%~5.22%), and the bluish dogbane degummed ramie finish fineness obtained is thin (for 3.3~4.5dtex), fibre strength index good (for 3.9~7.6cN/dtex), (average length is big for average fiber length length In 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, production efficiency is high, production cost is greatly reduced.
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 hermetically sealed can, is immersed in the ethylenediamine that mass percent concentration is 40%, in room temperature It persistently stirs 12 hours down, so that the infiltration activation of bluish dogbane bast;
Then, ethylenediamine in tank is vented, takes out the bluish dogbane bast by infiltration activation.
Bluish dogbane raw material after ethylenediamine infiltration activation is directly placed into steam explosion device, heating makes steam explosion fill Water vapour pressure in setting is 0.8MPa, keeps this pressure 1 minute;Then valve, rapid pressure release are opened;
The apocynum fibre sprayed from steam explosion equipment is collected, then carries out buying cake, it is tough that bluish dogbane obtained by cake will be beaten Skin and numb cage are placed in glue kettle together, are pumped into the FeSO that mass percent concentration is 0.05%4Solution, until it is tough not cross bluish dogbane Skin makes FeSO using high-pressure pump at room temperature4Solution inner-outer circulation 15 minutes empties FeSO4After solution, it is pumped into mass percent After emptying hydrogen peroxide solution, it is dense to be pumped into mass percent in 30 DEG C of circular treatments 1 hour for a concentration of 0.5% hydrogen peroxide solution Degree is 0.1% sodium hydroxide solution, boils and boils 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 bluish dogbane 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 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 hermetically sealed can, the solvent dimethylformamide that mass percent concentration is 60% is immersed in In, it is continuously stirred at room temperature 20 hours, so that the infiltration activation of bluish dogbane bast;
Then, dimethylformamide in tank is vented, takes out the bluish dogbane bast by infiltration activation.
Dimethylformamide is infiltrated and is activated
Bluish dogbane raw material afterwards is directly placed into steam explosion device, and heating makes the water vapour pressure in steam explosion device For 1.2MPa, this pressure is kept 5 minutes;Then valve, rapid pressure release are opened;
The apocynum fibre sprayed from steam explosion equipment is collected, then carries out buying cake, it is tough that bluish dogbane obtained by cake will be beaten Skin and numb cage are placed in glue kettle together, are pumped into the FeCl that mass percent concentration is 0.1%2Solution, until it is tough not cross bluish dogbane Skin makes FeCl using high-pressure pump at room temperature2Solution inner-outer circulation 30 minutes empties FeCl2After solution, it is pumped into mass percent A concentration of 2.5% peracetic acid soln after emptying peracetic acid soln, was pumped into quality percentage in 50 DEG C of circular treatments 1 hour The sodium hydroxide solution that specific concentration is 0.1%, boiling are boiled 0.5 hour.
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 bluish dogbane 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 3.3dtex.
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, using carbamide peroxide solution substitute hydrogen peroxide, using dimethylacetylamide replace ethylenediamine, the matter of carbamide peroxide solution It is except 1.5% to measure percent concentration;
Remaining, with embodiment 1.
Examination and test of products testing result:
Obtained bluish dogbane 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 4.0dtex.
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 bluish dogbane degummed ramie, 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 hermetically sealed can, 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 the infiltration activation of bluish dogbane bast;
Then, by organic amine solvent vent in tank, the bluish dogbane bast by infiltration activation is taken out, it is spare;
Second step dodges quick-fried activation process step
It by the bluish dogbane bast after infiltration activates, is placed in steam explosion device, is passed through steam, until steam explosion device The pressure of interior vapor reaches 0.8~1.2MPa, and pressurize 1~5 minute at this pressure;
Then, rapid pressure release is dodged quick-fried, obtains the bluish dogbane bast of dispersion activation;
Third walks, and beats cake dress cage step
By in the numb cage of bluish dogbane bast feeding of gained dispersion activation, cake is beaten using pancake making machine;Feed fiber crops when, 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;
4th step, 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- In glue tank activator bath foam always with swiftly flowing state constant impingement bluish dogbane bast 1~2 hour after, stop high-pressure pump, close 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;
5th 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;
6th step, post-processing step
By obtained apocynum fibre semi-finished product successively through being dehydrated, oiling, dry to get bluish dogbane degummed ramie finished product.
2. the fine design method of bluish dogbane degummed ramie according to claim 1, which is characterized in that the organic amine Solvent is one or more of ethylenediamine, dimethylformamide or dimethylacetylamide.
3. the fine design method of bluish dogbane degummed ramie according to claim 1, which is characterized in that the ferrous salt is molten Liquid is FeSO4Solution or FeCl2Solution, mass percent concentration are 0.03%~1%.
4. the fine design method of bluish dogbane degummed ramie according to claim 1, which is characterized in that the activator bath 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 any bluish dogbane degummed ramies of claim 1-4, which is characterized in that the alkali Property 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 bluish dogbane degummed ramies of claim 1-4, which is characterized in that obtained Bluish dogbane degummed ramie finished product 3.3~4.5dtex of fineness, residual gum content be 3.68%~5.22%, fibre strength be 3.9~ The average length of 7.6cN/dtex, fiber are more than 35mm.
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