CN106567136A - Fine production method of apocynum venetum fibers - Google Patents

Fine production method of apocynum venetum fibers Download PDF

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Publication number
CN106567136A
CN106567136A CN201610953752.9A CN201610953752A CN106567136A CN 106567136 A CN106567136 A CN 106567136A CN 201610953752 A CN201610953752 A CN 201610953752A CN 106567136 A CN106567136 A CN 106567136A
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bast
apocyni veneti
herba apocyni
sodium
liquid
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CN106567136B (en
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张元明
韩光亭
高守武
王聪儿
宋焱
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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
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01BMECHANICAL TREATMENT OF NATURAL FIBROUS OR FILAMENTARY MATERIAL TO OBTAIN FIBRES OF FILAMENTS, e.g. FOR SPINNING
    • D01B1/00Mechanical separation of fibres from plant material, e.g. seeds, leaves, stalks
    • D01B1/10Separating vegetable fibres from stalks or leaves
    • D01B1/14Breaking or scutching, e.g. of flax; Decorticating

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Molecular Biology (AREA)
  • Wood Science & Technology (AREA)
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  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention discloses a fine production method of apocynum venetum fibers. The production method includes the steps of: steam-cooking bast of apocynum venetum and removing impurities, performing steam explosion activation treatment, shaping the apocynum venetum bast into cake and placing the apocynum venetum bast in cages; performing oriented catalytic oxidization; and performing chemical degumming and after-treatment. After the steam explosion activation treatment, the oriented catalytic oxidization is carried out to lignin and semi-cellulose by means of a copper salt solution and an activator. Through organic combination of technical means such as the steam explosion degumming treatment and the oriented catalytic oxidization, the production method is good in degumming effect. An apocynum venetum fiber finish product is good in indices such as fineness, length, strength and the like, has high quality and good spinnability. In addition, the method is low in chemical substance consumption quantity and is low in environment-protective stress, is easy to control, is low in consumption on utilities such as water, electricity and steam, and is suitable for industrial production.

Description

A kind of production method that becoming more meticulous of apocynum fibre
Technical field
The present invention relates to a kind of processing method of flaxen fiber, more particularly to a kind of producer that becomes more meticulous of apocynum fibre Method.
Background technology
Herba Apocyni veneti, also known as wild flax, Herba Euphorbiae Helioscopiae fiber crops, red building, apocynum cannabinum etc., are a kind of perennial herb plants, category Apocynaceae, is widely distributed in the northern area of China, and Tarimhe River and Kongquehe of the integrated distribution in Xinjiang is littoral, because its Spread out Plain growth and most contain and gain the name in Xinjiang.Apocynum fibre has many excellent characteristics, soft and good luster, with silk Gloss, the very light of fiber crops, the softness of cotton, the malleability of floss, and have pharmacological action were 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 located in the phloem tissue on Herba Apocyni veneti plant stem, in fibre bundle Shape, individuals fibers individualism.Herba Apocyni veneti ultimate fibre is that a kind of two end seal closes have in the middle part of the ﹑ of born of the same parents chamber thick and two ends thin in the middle of ﹑ thin Born of the same parents' shape object, in obvious irregular kidney-shaped, lumen is less in section, and without torsion, there are many vertical lines on surface have for fiber longitudinal direction Horizontal section is present.Fibre fineness is about 3~4dtex, and length is 20~25mm, and fiber width is 10~50 μm.
The chemical composition of Herba Apocyni veneti bast has certain difference with other bast-fibres.Herba Apocyni veneti bast hemicellulose level 16.31%, content of lignin 12.09% is above Zhu Ma ﹑ Ya Ma ﹑ Fructus Cannabiss, and especially content of lignin is apparently higher than other fiber crops Class, and content of cellulose be only 45.74% be minimum in all bast-fibres.
Due to Herba Apocyni veneti bast non-cellulose components it is high, up to nearly the 55% of Herba Apocyni veneti bast, especially hemicellulose and Content of lignin is high, more than the 28% of Herba Apocyni veneti bast.Therefore, apocynum degumming is increasingly difficult compared with other bast-fibres, tradition Bast-fibre Degumming method be not appropriate for the degumming process of apocynum fibre, it is necessary to select to take off with reference to Herba Apocyni veneti own characteristic Gluing method and technique.
In prior art, conventional apocynum fibre Degumming method is main or the chemical method of traditional bast-fibre degumming, Bioanalysises or Physical.Wherein, because causing waste water to be difficult to process using a large amount of chemical reagent, environmental pollution is serious for chemical method, takes off Hot conditionss energy consumption cost needed for glue is high, at the same chemical Degumming be difficult to Proper Match fibre strength, between length and fineness Relation, degumming excessively causes 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 little, cohesive force is poor, and the limit count of yarn is low, and wiriness, filoplume are more, and prodding and itching feeling is strong, The premium properties of apocynum fibre can not be fully demonstrated, the range of application of apocynum fibre is seriously limited.
For bioanalysises, many bioenzyme activities are not enough, be generally difficult to be applied to apocynum fibre internal component it is complicated, Compact structure part, is especially difficult to remove lignin portion, therefore bioanalysises are present, and degumming quality is unstable, efficiency is low, consumption The problems such as duration, high cost, major part, are 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, application is the most general It is steam explosion technology all over be.But, in the steam explosion processing procedure about research report, vapor (steam) temperature is high, pressure is big, Particularly, multiple repetition exploding technology is generally required, inevitably, apocynum fibre strength damage and fiber will be caused long Degree loss.
In a word, for the high feature of lignin and hemicellulose level in Herba Apocyni veneti bast raw material, not to Herba Apocyni veneti In the case that raw material carries out pretreatment, by during single chemistry, biology or physics effect degumming, processing conditionss are difficult to Control, fibre strength are difficult to rationally control with length, fineness relation, or processing gained apocynum fibre is 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 its effectively utilizes, 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 of the softening and textile for concentrating on fiber mostly, Without solve fiber itself the problem that becomes more meticulous, simply softening fibre and reduce fibre-fibre friction power, this is obviously to Herba Apocyni veneti Product is lightening and superior has little significance.
The apocynum fibre of low damage becomes more meticulous production method, is the key for lifting apocynum fibre value, represents The trend and direction of industry technology development.
The content of the invention
It is an object of the present invention to provide a kind of production method that becomes more meticulous of apocynum fibre, to overcome the de- of prior art The apocynum fibre that time-consuming for gluing method generally existing, chemical drugss usage amount is big, prepared is short, thick, hard, low strength Etc. technical problem.
The technical scheme that adopted for achieving the above object of the present invention is, a kind of producer that becomes more meticulous of apocynum fibre Method, it is characterised in that comprise the following steps:
The first step, the steaming and decocting removal step of Herba Apocyni veneti bast
Herba Apocyni veneti bast is placed in rotary spherical digester, digester or cooker, injection cooking liquor is until by Herba Apocyni veneti bast submergence Under steaming and decocting liquid level;Heating cooking liquor is to boiling, steaming and decocting 0.5~1 hour under fluidized state, to carry out Herba Apocyni veneti bast remove impurity Process;
Then, the Herba Apocyni veneti bast processed through remove impurity is taken out, it is standby;
The cooking liquor is the mixed aqueous solution of surfactant and metal ion chelation agent, wherein, surfactant Mass percent concentration is 0.1%~2%, and the mass percent concentration of metal ion chelation agent is 0.3%~0.5%;
Above-mentioned surfactant is sulfated castor oil, dodecyl sodium sulfate, sodium lauryl sulphate, detergent alkylate Sodium sulfonate, dioctyl sodium sulfosuccinate, Laurel alcohol sulfuric ester MA24F, SAS SAS60, pull open point, rapid osmotic One kind in agent T, penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10 or N- ethyl pyrrolidone NEP-100 or It is various;
Above-mentioned metal ion chelation agent is sodium tripolyphosphate, sodium hexameta phosphate, sodium pyrophosphate, sodium silicate, sodium citrate, benzene One or more in sodium formate, polyacrylamide, sodium salicylate or tetrasodium ethylenediamine tetraacetate;
Second step, dodges quick-fried activation process step
By the Herba Apocyni veneti bast after remove impurity is processed, it is placed in steam explosion device, is passed through steam, until steam explosion In device, the pressure of vapor reaches 1.0~1.5MPa, and pressurize 1~5 minute at this pressure;
Then, rapid pressure release dodges quick-fried, then with clear water washes clean after, obtain disperseing the Herba Apocyni veneti bast of activation;
3rd step, beats cake dress cage step
Gained is disperseed, in the numb cage of Herba Apocyni veneti bast feeding of activation, to buy cake using pancake making machine;When feeding fiber crops, numb cage is with 3~5 Rev/min speed do not stop rotation, 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 continuously spraying water into numb cage, 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 for being loaded with Herba Apocyni veneti bast is integrally placed in glue kettle, is opened liquid feed valve, is made First copper salt solution to liquid level is injected into glue kettle with high-pressure pump do not had Herba Apocyni veneti bast;
Then, continue to keep high-pressure pump operating, so that copper salt solution and outside copper salt solution forced circulation in glue kettle, protect Hold copper salt solution in glue kettle and, all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast, after 15~30 minutes, stop high pressure Pump, closing liquid feed valve, opening liquid valve, will close liquid valve after the copper salt solution emptying in glue kettle;
Then, liquid feed valve is opened, activator body lotion is injected into glue kettle using high-pressure pump is first, until liquid level and do not spread out Numb bast;Then, continue to keep high-pressure pump operating, so that activator body lotion is forced to follow with external activator body lotion in glue kettle Ring, keeps in glue kettle activator body lotion all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast, 1.5~2.5 hours Afterwards, stop high-pressure pump, close liquid feed valve, open liquid valve, liquid valve will be closed after the activator body lotion emptying in glue kettle;
Above-mentioned activator is H2O2, peracetic acid or carbamide peroxide solution;
5th step, chemical Degumming step
Then, liquid feed valve is opened, alkaline degumming liquid is pumped into into glue kettle, did not had Herba Apocyni veneti bast to liquid level, heating is boiled Boiling, and continuously cooking 0.5~2 hour under fluidized state;
Then, degumming liquid is emptied, injection sulphuric acid or hydrochloric acid body lotion wash Herba Apocyni veneti bast to pH value≤7;Reuse clear Water rinsed clean repeatedly, obtains apocynum fibre semi-finished product;
6th step, post-processing step
Resulting apocynum fibre semi-finished product successively Jing are dehydrated, oil, are dried, apocynum fibre finished product is obtained final product.
Preferably, above-mentioned copper salt solution is CuSO4Solution, CuCl2Solution or Cu (NO3)2Solution, mass percent concentration It is 0.03%~1%.
Further preferably, the mass percent concentration 0.5%~2.5% of above-mentioned activator body lotion, pH value are 3~5, temperature For 30 DEG C~50 DEG C;Bath raio is 1:10.
Further preferably, above-mentioned alkaline degumming liquid is sodium hydroxide solution that mass percent concentration is 0.1%~1%; Or, the body lotion for making as follows:Sodium hydroxide is added in used steaming and decocting remove impurity waste liquid, so that therein The mass percent concentration of sodium hydroxide reaches 0.1%~1% body lotion;
The mass percent concentration of the sulphuric acid or hydrochloric acid body lotion is 0.1%, and bath raio is 1:20.
Further preferably, the production method that becomes more meticulous of above-mentioned apocynum fibre, it is characterised in that obtained Herba Apocyni veneti The fineness of fibrous finished product is 3.2~4.6dtex, and residual gum content is 3.68%~5.22%, and fibre strength is 3.8~7.8cN/ Dtex, the average length of fiber are more than 35mm.
What above-mentioned technical proposal 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 3.2~4.6dtex), fibre strength index are good (for 3.8~7.8cN/ Dtex), fabric (average length is more than 35mm) of fine quality;
The production method that becomes more meticulous of the apocynum fibre of above-mentioned technical proposal, in whole production process, chemical cost amount Little, environmental protection pressure mitigates, and technique controlling difficulty is greatly reduced;The utility consumptions such as water power vapour are little, production efficiency is high, production Low cost.
To more fully understand the technical characterstic of the present invention, show labor and be described as follows:
In above-mentioned technical proposal, Herba Apocyni veneti bast raw material is carried out into steaming and decocting remove impurity, sieve is can remove in steaming and decocting dedoping step Cloth fiber crops bast in most of hydrotrope and part hemicellulose (the part hemicellulose on Herba Apocyni veneti bast, at high temperature, can Generation hydrolysis and be removed), and then reduce subsequent chemistry reagent consumption and consumption.
Meanwhile, in steaming and decocting dedoping step, under the infiltration, wetting action in high temperature and surfactant, Herba Apocyni veneti can be softened The sclerderm on bast top layer, removes beneficial to following process.
What is more important, in steaming and decocting removal step, under surfactant infiltration, moistening, dispersion and emulsification, can Original most of inorganic matters in Herba Apocyni veneti bast raw material are rapidly removed, easily absorption, complexation or chelating Cu is especially can remove2+ The impurity of ion, the Cu added in preventing follow-up directional catalyzing oxidation step2+Ion " is inactivated ".
In addition, under surfactant infiltration, moistening, dispersion and emulsification, can quickly remove Herba Apocyni veneti bast raw material In original most of oily matter, strengthen the wellability of Herba Apocyni veneti bast, spread out in improving follow-up directional catalyzing oxidation step Numb bast is to Cu2+The adsorption efficiency of ion.
Meanwhile, under the chelation of metal ion chelation agent, steaming and decocting removal step can effectively remove Herba Apocyni veneti bast institute The metal cation component for containing, so as to the catalytic decomposition for being prevented effectively from the activator that these metal cation components are likely to result in is anti- Should.That is, better ensure that the effect of follow-up directional catalyzing oxidation.
In above-mentioned technical proposal, the Herba Apocyni veneti bast after steaming and decocting remove impurity is processed is carried out into steam explosion activation processing, In the process, the vapor and aqueous water of high-temperature high-pressure state acts on Herba Apocyni veneti raw material, raw material is carried out fully swelling;So Afterwards, in the presence of moment pressure release, Herba Apocyni veneti bast is loosened or is disperseed, realize the activation processing of Herba Apocyni veneti bast.
The water-washing step of quick-fried activation process step in above-mentioned technical proposal, is dodged, glue during steam explosion can be directly removed Matter is degraded generated small molecule and partly drops poly- macromole colloid, reduces the consumption of subsequent processing steps chemicals;More Importantly, water-washing step can effectively remove the metal ion-chelant of brought into Herba Apocyni veneti bast in Herba Apocyni veneti bast digestion process Agent, prevents the Cu in directional catalyzing oxidation step2+Ion " is inactivated ".
In above-mentioned technical proposal, beat during cake using while beat cake, while hot water spray method, to the quick-fried activation processing of Jing sudden strains of a muscle Herba Apocyni veneti bast carry out buying cake, the colloid in Herba Apocyni veneti bast can be made further to soften under the action of soaking of warm water, and Partly remove in the presence of mechanical force;Especially, act on warm water process as mechanical external force is acted on during buying cake, can be effective The part Herba Apocyni veneti bast top layer sclerderm of the be difficult to removal of subsequent handling is removed, and then following process can be greatly reduced and process strong Degree, and the consumption of chemical reagent.
It is important to note that in above-mentioned technical proposal, in directional catalyzing oxidizing process, loosening Jing after dodging quick-fried activation Or the hemicellulose and lignin Adsorption of Cu in the presence of oxy radical on scattered Herba Apocyni veneti bast surface2+
After adding activator, Cu is adsorbed with2+Hemicellulose and lignin take the lead in be oxidized degraded, part be oxidized degraded Removal is directly dissolved for small organic molecule, be partly oxidized to the material that subsequent chemistry degumming is more easy to remove.
In directional catalyzing oxidation step, Adsorption of Cu2+Herba Apocyni veneti bast, without washing, that is, be placed directly within containing activator Solution in, it is therefore an objective to protect Cu2+Directional catalyzing activator decomposes, and then oxidative lignin and hemicellulose, strengthens catalysis oxygen Change effect.
In above-mentioned technical proposal, in chemical Degumming step, degumming liquid is by adding hydroxide using steaming and decocting remove impurity waste liquid The alkaline degumming liquid that sodium is prepared, can reduce the usage amount of fresh water, reduce quantity of wastewater effluent.
In addition, steaming and decocting remove impurity waste liquid sheet is as hot water, it is re-used for chemical Degumming step and can reduces whole technical process Energy consumption.What is more important, as steaming and decocting remove impurity waste liquid itself contains surfactant, directly utilizes to which, can avoid chemistry The addition again of surfactant in degumming step, reduces the consumption of whole technical process chemicals, increases making for chemicals Use efficiency.
Wherein, activated and Cu using steam explosion2+Ion and hydrogen peroxide (or peracetic acid or carbamide peroxide solution) It is one of key problem in technology point of the present invention that immersion is oriented catalytic oxidation treatment to Herba Apocyni veneti bast, fine to final Herba Apocyni veneti Dimension treatment effect serves very crucial effect.Reason is as follows:
In Herba Apocyni veneti phloem, bonding of the apocynum fibre cellulose fiber element in colloids such as pectin, hemicellulose and lignins Lower bunchy (technique) fiber is acted on, wherein ultimate fibre length is 20~25mm, and diameter is then 10~50 μm, colloid (pectin, half fibre Dimension 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 fiber Centre is enclosed in outside fiber, defines the Network Three-dimensional space structure of densification so that cellulosic sections are difficult dispersion.Traditional Degumming method is all the effect by chemical reagent or enzyme, is successively stripped down the colloid in bundle fiber from outside to inside, Cause degumming degree inside and outside raw material inconsistent, outer layer degumming degree is better than internal layer, cause end article quality decline, while this mistake Journey reaction condition is wayward, if degumming effect is violent, fiber can be caused to shorten, weaving use value is lost;If degumming is imitated Really bad, residual gum content is higher, and fiber will be caused thick, hard, rough, is equally unfavorable for that follow-up textile process operation is used.
Therefore, to change the degumming mode for successively peeling off colloid from outside to inside, with condition Proper Match sieve of milder Cloth fiber crops process of fiber intensity, the relation between fineness, length, need the orientation that part non-cellulosic material is carried out to raw material to remove.
And the steam explosion activation processing of above-mentioned technical proposal, because steam explosion processes low intensity, so, can not destroy In the case of apocynum fibre bulk composition cellulosic degree of polymerization, in destruction raw material in the component molecules such as lignin, hemicellulose And the hydrogen bond between intermolecular and lignin, hemicellulose and cellulosic molecule, reduction colloid and colloid and colloid and fiber The adhesion of element, while increase the swollen degree of raw material, partial removal hemicellulose and lignin, beneficial to subsequent chemistry reagent Infiltration is simultaneously further had an effect.
Meanwhile, in the steam explosion activated process of above-mentioned technical proposal, high temperature, the vapor of high pressure conditions and liquid Water acts on Herba Apocyni veneti raw material, and abundant swollen is carried out to raw material, in subsequent moment pressure leak process, class mechanical disintegration act on, Under hydrogen bond destruction and the synergy of structural rearrangement, between hemicellulose and hemicellulose, hemicellulose and lignin Between, connection between hemicellulose and cellulose, between lignin and cellulose fracture or weaken, raw material loosened or point Dissipate, increase Herba Apocyni veneti bast raw material specific surface area, follow-up Cu can be strengthened2+The absorption of ion.Meanwhile, in steam explosion process In, in the presence of class acidic hydrolysises and thermal degradation, remove can part hemicellulose degradation, reduce following process and process strong Degree 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 or decrease between cellulose, between lignin and cellulose, makes Herba Apocyni veneti raw material be loosened or be disperseed, makes original While material specific surface area increases, as the colloids such as hemicellulose and lignin are wrapped in fibrous outer, stock chart is thus in The hemicellulose in face and content of lignin increase, and make more groups containing O be exposed to raw material surface, contain in hemicellulose and lignin In the presence of O electron-donating groups, can the more Cu of active adsorption2+Ion, enhances Herba Apocyni veneti bast raw material Cu2+Ionic adsorption Activity, beneficial to Cu in follow-up orientation activation process2+The absorption of ion, and then be conducive to the carrying out of follow-up directional catalyzing oxidation.
In addition, in quick-fried activation process is dodged, the vapor and aqueous water of high-temperature high-pressure state can well to being difficult to remove Herba Apocyni veneti bast crust carry out effective swollen, in subsequent moment pressure leak process class mechanical disintegration effect under, by itself and sieve The tough endo-endothelial layer of cloth fiber crops is separated and is removed, and is reduced difficulty and intensity that follow-up directional catalyzing oxidation and soda boiling are processed, is reduced follow-upization Learn the usage amount of reagent.
Meanwhile, in quick-fried activation process is dodged, in the joint of the effect of class mechanical disintegration, hydrogen bond destruction and structural rearrangement Under effect, Herba Apocyni veneti bast raw material has been obtained effectively loosening or has been disperseed, and is taken off with the chemical Degumming method and biology of 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 oxidizing process, Jing dodges the Herba Apocyni veneti raw material of quick-fried activation processing, due to hemicellulose and lignin Surface oxygen-containing groups increase, in CuSO4、CuCl2Or Cu (NO3)2Under the immersion of solution, Herba Apocyni veneti raw material surface is adsorbed in a large number Cu2+, then in hydrogen peroxide or peracetic acid or carbamide peroxide solution are processed, the Cu of hemicellulose and lignin absorption2+ The H that hemicellulose and lignin surface catalysis directly add2O2Or the H that peracetic acid or the hydrolysis of carbamide peroxide solution are generated2O2 Decompose, in acid condition, Cu2+Catalysis H2O2Decompose and produce the extremely strong HO of oxidability, due to the oxidability pole for producing Strong HO is predominantly located at hemicellulose and lignin surface, therefore can be degraded to part hemicellulose water soluble little Molecular organic and be dissolved in the water;Simultaneously because HO oxidabilities are extremely strong, can by complex structure and be difficult to remove it is wooden There is ring-opening reaction in plain side chain C-C bond fissions, generate the structure that subsequent chemistry degumming is more easy to remove, it is easy to which follow-up degumming is gone Remove.While HO Oxidation radius very littles, and as cellulose is wrapped in hemicellulose and lignin, therefore the oxygen of HO Change effect is difficult to make cellulose oxidation degrade.
During chemical Degumming, high temperature alkaline solution can hydrolyze the remaining most non-cellulosic material of removal, especially may be used There are hydrolysis and remove in the lignin for making oxidized rear side chain C-C bond fissions or ring-opening reaction occurring so that fiber enters one Step dispersion, the brilliant effect while cellulose disappears under alkali liquor, reduces degree of crystallinity, improves the hydrophilic of fiber, softening fibre.
In above-mentioned technical proposal, why by the Herba Apocyni veneti bast raw material aoxidized through directional catalyzing, without the need for washing, that is, exist After emptying reactant liquor, being pumped directly into alkali liquor carries out degumming process, it is therefore intended that, remaining, undecomposed activator can increase alkali Boil the degumming effect and bleaching effect in scouring processes.
Certainly, pre- acid treatment correspondingly, with prior art, pre- alkali process, pre- urine oxygen process chemical Degumming method contrast, Before chemical Degumming, a water-washing step is eliminated, water consume is reduced.
Meanwhile, the chemical Degumming method ratio with prior art, above-mentioned technical proposal need not move through the length of a large amount of chemical reagent Time steaming and decocting, by Cu under steam explosion and acid condition2+The selective paraffin oxidation degraded of the HO that ionic catalysises activator is produced is made There is efficiency high, the significant advantage such as little is polluted with apocynum fibre degumming is carried out.
In above-mentioned technical proposal, pickling prevents alkali from entering one to cellulose then in order to neutralize the alkaline reagent of chemical Degumming Step degraded;Oil to improve the apparent condition of fiber, increase the laxity and softness of fiber, be easy to follow-up spinning.
In a word, just because of the combination of above-mentioned series technique means so that in apocynum fibre crude product alkaline boiling, Process compared with the steaming and decocting of prior art, the time required to chemical levels, steaming and decocting, aspect is greatly decreased or saves, 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 is respectively provided with obvious positive effect.
Supplementary notes:In above-mentioned technical proposal, the apocynum fibre after alkaline scouring process, remaining colloid in fiber And pigment, further removed, so as to reach ideal flax fiber separation index and whiteness index.
In sum, the present invention is had the advantages that relative to prior art:
1st, on the basis of obtaining compared with the more preferable degumming effect of prior art (residual gum content is 3.68%~5.22%), obtained Apocynum fibre finish fineness thin (being 3.2~4.6dtex), fibre strength index good (being 3.8~7.8cN/dtex), fine Dimension average length length (average length is more than 35mm), good spinnability;
2nd, chemical cost amount is little, environmental protection pressure mitigates, and technique controlling difficulty is greatly reduced;
3rd, the utility consumption such as water, electricity, vapour is little, improve production efficiency, reduce production cost.
Specific embodiment
With reference to 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 rotary spherical digester or digester or cooker, is immersed in cooking liquor, is heated to fluidized state, Steaming and decocting 0.5 hour, carries out Herba Apocyni veneti bast remove impurity.
Herba Apocyni veneti raw material after steaming and decocting remove impurity is directly placed in steam explosion device, heating is made in steam explosion device Water vapour pressure is 1.0MPa, keeps this pressure 1 minute;Then valve, rapid pressure release are opened;
The apocynum fibre that sprays from steam explosion equipment of collection, then carries out buying cake, will beat Herba Apocyni veneti obtained by cake it is tough Skin and numb cage are together placed in glue kettle, pump into the CuSO that mass percent concentration is 0.05%4Solution, to not having Herba Apocyni veneti tough Skin, at room temperature, makes CuSO using high-pressure pump4Solution inner-outer circulation 15 minutes, empties CuSO4After solution, mass percent is pumped into Concentration is 0.5% hydrogen peroxide solution, after 30 DEG C of circular treatment 1.5 hours, emptying hydrogen peroxide solution, pumps into mass percent Concentration is 0.1% sodium hydroxide solution, and boiling boils 1 hour.
Then, carry out pickling to the fiber after steaming and decocting at room temperature, pickle is the sulfur that mass percent concentration is 0.1% (acid cleaning process selects bath raio to be 1 for acid or solution:20), pickling time is 5 minutes.
It is neutrality by fiber washing to pH value, finally, successively Jing after being dehydrated, oil, dry, obtains final product fine Herba Apocyni veneti fine Dimension.
Above-mentioned cooking liquor is the mixed aqueous solution of surfactant and metal ion chelation agent, wherein, surfactant Mass percent concentration is 0.1~2%, and the mass percent concentration of metal ion chelation agent is 0.3~0.5%;
Above-mentioned surfactant is sulfated castor oil;
Above-mentioned metal ion chelation agent is sodium tripolyphosphate.
Examination and test of products testing result:
Obtained apocynum fibre residual gum content is 5.22%, and average fiber length is more than 35mm, and fibre strength is 7.8cN/dtex, fibre fineness are 4.6dtex.
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 rotary spherical digester or digester or cooker, is immersed in cooking liquor, is heated to fluidized state, Steaming and decocting 0.5 hour, carries out Herba Apocyni veneti bast remove impurity.
Herba Apocyni veneti raw material after steaming and decocting remove impurity is directly placed in steam explosion device, heating is made in steam explosion device Water vapour pressure is 1.5MPa, keeps this pressure 5 minutes;Then valve, rapid pressure release are opened;
The apocynum fibre that sprays from steam explosion equipment of collection, then carries out buying cake, will beat Herba Apocyni veneti obtained by cake it is tough Skin and numb cage are together placed in glue kettle, pump into the CuCl that mass percent concentration is 0.1%2Solution, to not having Herba Apocyni veneti tough Skin, at room temperature, makes CuCl using high-pressure pump2Solution inner-outer circulation 30 minutes, empties CuCl2After solution, mass percent is pumped into Concentration is 2.5% peracetic acid soln, after 50 DEG C of circular treatment 1.5 hours, emptying peracetic acid soln, pumps into quality hundred The sodium hydroxide solution that specific concentration is 0.1%, boiling is divided to boil 0.5 hour.
Then, carry out pickling to the fiber after steaming and decocting at room temperature, pickle is the salt that mass percent concentration is 0.1% (acid cleaning process selects bath raio to be 1 to acid solution:20), pickling time is 5 minutes.
It is neutrality by fiber washing to pH value, finally, successively Jing after being dehydrated, oil, dry, obtains final product fine Herba Apocyni veneti fine Dimension.
Above-mentioned cooking liquor is the mixed aqueous solution of surfactant and metal ion chelation agent, wherein, surfactant Mass percent concentration is 0.1~2%, and the mass percent concentration of metal ion chelation agent is 0.3~0.5%;
Above-mentioned surfactant is sulfated castor oil;
Above-mentioned metal ion chelation agent is sodium tripolyphosphate.
Examination and test of products testing result:
Obtained apocynum fibre residual gum content is 3.68%, and average fiber length is more than 35mm, and fibre strength is 3.8cN/dtex, fibre fineness are 3.2dtex.
Embodiment 3
The Herba Apocyni veneti bast places of origin of raw materials:Xinjiang
Processing method:Except CuSO4Solution quality percent concentration is that the time of 1%, alkaline degumming liquid continuously cooking is little for 2 When, substitute hydrogen peroxide using carbamide peroxide solution, the mass percent concentration of carbamide peroxide Solutions Solution be 1.5% it Outward;
Remaining, with embodiment 1.
Examination and test of products testing result:
Obtained apocynum fibre residual gum content is 4.62%, and average fiber length is more than 35mm, and fibre strength is 6.2cN/dtex, fibre fineness are 3.9dtex.
It is pointed out that above-mentioned surfactant is also possible that such as:Dodecyl sodium sulfate, lauryl sulphate acid Sodium, dodecylbenzene sodium sulfonate, dioctyl sodium sulfosuccinate, Laurel alcohol sulfuric ester MA24F, SAS SAS60, drawing Open powder, fast penetrant T, penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10, N- ethyl pyrrolidone NEP- 100;
Or, including any two kinds of sulfated castor oil, dodecyl sodium sulfate and the above surfactant The mixture (mixed proportion does not have particular/special requirement, can the factor such as integrated cost carry out reasonable selection) of above composition.
Above-mentioned metal ion chelation agent is also possible that such as:Sodium hexameta phosphate, sodium pyrophosphate, sodium silicate, sodium citrate, benzene Sodium formate, polyacrylamide, sodium salicylate, tetrasodium ethylenediamine tetraacetate;
Or, including any two kinds of sodium tripolyphosphate, sodium hexameta phosphate and the above metal ion chelation agent with The mixture (mixed proportion does not have particular/special requirement, can the factor such as integrated cost carry out reasonable selection) of upper composition.

Claims (5)

1. the production method that becomes more meticulous of a kind of apocynum fibre, it is characterised in that comprise the following steps:
The first step, the steaming and decocting removal step of Herba Apocyni veneti bast
Herba Apocyni veneti bast is placed in rotary spherical digester, digester or cooker, injection cooking liquor is until be immersed in steaming by Herba Apocyni veneti bast Under boil liquid face;Heating cooking liquor to seething with excitement, steaming and decocting 0.5~1 hour under fluidized state, to carry out Herba Apocyni veneti bast except living together Reason;
Then, the Herba Apocyni veneti bast processed through remove impurity is taken out, it is standby;
The cooking liquor is the mixed aqueous solution of surfactant and metal ion chelation agent, wherein, the quality of surfactant Percent concentration is 0.1%~2%, and the mass percent concentration of metal ion chelation agent is 0.3%~0.5%;
Above-mentioned surfactant is sulfated castor oil, dodecyl sodium sulfate, sodium lauryl sulphate, DBSA Sodium, dioctyl sodium sulfosuccinate, Laurel alcohol sulfuric ester MA24F, SAS SAS60, pull open point, fast penetrant T, One or more in penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10 or N- ethyl pyrrolidone NEP-100;
Above-mentioned metal ion chelation agent is sodium tripolyphosphate, sodium hexameta phosphate, sodium pyrophosphate, sodium silicate, sodium citrate, benzoic acid One or more in sodium, polyacrylamide, sodium salicylate or tetrasodium ethylenediamine tetraacetate;
Second step, dodges quick-fried activation process step
By the Herba Apocyni veneti bast after remove impurity is processed, it is placed in steam explosion device, is passed through steam, until steam explosion device The pressure of interior vapor reaches 1.0~1.5MPa, and pressurize 1~5 minute at this pressure;
Then, rapid pressure release dodges quick-fried, then with clear water washes clean after, obtain disperseing the Herba Apocyni veneti bast of activation;
3rd step, beats cake dress cage step
Gained is disperseed, in the numb cage of Herba Apocyni veneti bast feeding of activation, to buy cake using pancake making machine;Feed fiber crops when, numb cage with 3~5 turns/ The speed of minute does not stop rotation, and pancake making machine machinery foot moves up and down to beat and beats Herba Apocyni veneti bast in fact;Meanwhile, watering duckbilled is from up to Lower drip washing of continuously spraying water into numb cage, 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 for being loaded with Herba Apocyni veneti bast is integrally placed in glue kettle, opens liquid feed valve, using height Press pump first into glue kettle injects copper salt solution to liquid level and did not had Herba Apocyni veneti bast;
Then, continue to keep high-pressure pump operating, so that copper salt solution and outside copper salt solution forced circulation in glue kettle, keep de- In glue tank, copper salt solution after 15~30 minutes, stops high-pressure pump, closes all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast Close liquid feed valve, open liquid valve, liquid valve will be closed after the copper salt solution emptying in glue kettle;
Then, liquid feed valve is opened, activator body lotion is injected into glue kettle using high-pressure pump is first, until liquid level did not had Herba Apocyni veneti tough Skin;Then, continue to keep high-pressure pump operating, so that activator body lotion and external activator body lotion forced circulation in glue kettle, protect Hold activator body lotion in glue kettle, all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast, after 1.5~2.5 hours, to stop High-pressure pump, closing liquid feed valve, opening liquid valve, will close liquid valve after the activator body lotion emptying in glue kettle;
Above-mentioned activator is H2O2, peracetic acid or carbamide peroxide solution;
5th step, chemical Degumming step
Then, liquid feed valve is opened, alkaline degumming liquid is pumped into into glue kettle, do not had a Herba Apocyni veneti bast to liquid level, heated and boiled, and Continuously cooking 0.5~2 hour under fluidized state;
Then, degumming liquid is emptied, injection sulphuric acid or hydrochloric acid body lotion wash Herba Apocyni veneti bast to pH value≤7;Reuse clear water anti- Multiple rinsed clean, obtains apocynum fibre semi-finished product;
6th step, post-processing step
Resulting apocynum fibre semi-finished product successively Jing are dehydrated, oil, are dried, apocynum fibre finished product is obtained final product.
2. the production method that becomes more meticulous of apocynum fibre according to claim 1, it is characterised in that the copper salt solution is CuSO4Solution, CuCl2Solution or Cu (NO3)2Solution, mass percent concentration are 0.03%~1%.
3. the production method that becomes more meticulous of apocynum fibre according to claim 1, it is characterised in that the activator body lotion Mass percent concentration be 0.5%~2.5%, pH value be 3~5, temperature be 30 DEG C~50 DEG C;Bath raio is 1:10.
4. the production method that becomes more meticulous according to the arbitrary described apocynum fibre of claim 1-3, it is characterised in that the alkalescence Degumming liquid is sodium hydroxide solution that mass percent concentration is 0.1%~1%;
Or, the body lotion for making as follows:
Sodium hydroxide is added in used steaming and decocting remove impurity waste liquid, so that the mass percent concentration of sodium hydroxide therein reaches To 0.1%~1% body lotion;
The mass percent concentration of the sulphuric acid body lotion or hydrochloric acid body lotion is 0.1%, and bath raio is 1 ︰ 20.
5. the production method that becomes more meticulous according to the arbitrary described apocynum fibre of claim 1-3, it is characterised in that obtained 3.2~the 4.6dtex of fineness of apocynum fibre finished product, residual gum content are 3.68%~5.22%, and fibre strength is 3.8~7.8cN/ Dtex, the average length of fiber are more than 35mm.
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JPS53111113A (en) * 1977-03-08 1978-09-28 Chiyouzou Hirao Method of finely spinning raw yarn and fabric
CN1924120A (en) * 2006-09-11 2007-03-07 东华大学 Method of preparing fiber for weave by peroxide degumming method
CN102586897A (en) * 2011-12-21 2012-07-18 中国热带农业科学院海口实验站 Method for preparing banana cellulose nanofibers by using steam explosion technology
CN102828255A (en) * 2012-08-24 2012-12-19 营口市新艺纺织有限责任公司 Processing method of long hemp
CN104047063A (en) * 2014-06-25 2014-09-17 江南大学 Method for preparing cotton stalk skin fiber for spinning with combination between steam explosion and alkali treatment
CN105256384A (en) * 2015-10-20 2016-01-20 东华大学 Method for oxidation degumming of ramie under weak acid condition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS53111113A (en) * 1977-03-08 1978-09-28 Chiyouzou Hirao Method of finely spinning raw yarn and fabric
CN1924120A (en) * 2006-09-11 2007-03-07 东华大学 Method of preparing fiber for weave by peroxide degumming method
CN102586897A (en) * 2011-12-21 2012-07-18 中国热带农业科学院海口实验站 Method for preparing banana cellulose nanofibers by using steam explosion technology
CN102828255A (en) * 2012-08-24 2012-12-19 营口市新艺纺织有限责任公司 Processing method of long hemp
CN104047063A (en) * 2014-06-25 2014-09-17 江南大学 Method for preparing cotton stalk skin fiber for spinning with combination between steam explosion and alkali treatment
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