CN106435756A - Refined production method for apocynum venetum fibers - Google Patents
Refined production method for apocynum venetum fibers Download PDFInfo
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- CN106435756A CN106435756A CN201610951963.9A CN201610951963A CN106435756A CN 106435756 A CN106435756 A CN 106435756A CN 201610951963 A CN201610951963 A CN 201610951963A CN 106435756 A CN106435756 A CN 106435756A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C1/00—Treatment of vegetable material
- D01C1/02—Treatment of vegetable material by chemical methods to obtain bast fibres
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/02—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
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Abstract
The invention discloses a refined production method for apocynum venetum fibers. The production method includes the steps: stewing apocynum venetum bast and removing impurities from the apocynum venetum bast; performing infiltrating and activating for the apocynum venetum bast by organic amine; performing steam explosion activating treatment; beating cakes and filling cages; performing orientation catalysis and oxidation; performing chemical gum removal and post-processing. After apocynum venetum bast is infiltrated and activated by the organic amine and activated by the aid of a steam explosion mode, lignin and hemi-cellulose are catalyzed and oxidized by the ferrous salt solution and activating agents in an oriented manner, a serials of technical means such as infiltrating and activating, steam explosion gum removal and orientation catalysis and oxidation are organically used, so that the production method has the advantages that the method is good in gum removal effect, obtained apocynum venetum fiber finished products are good in fineness, length, strength, quality and spinnability and the like, the production method is less in chemical consumption, low in environmental protection pressure, high in efficiency and applicable to industrial production, processes are simple to control, consumption of public works such as water, power and gas is less.
Description
Technical field
The present invention relates to a kind of production method of flaxen fiber, more particularly, to a kind of producer that becomes more meticulous of Herba Apocyni veneti degummed ramie
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, belong to
Apocynaceae, is widely distributed in the northern area of China, and the Tarimhe River in Xinjiang for the integrated distribution and Kongquehe are littoral, because its
Xinjiang is spreaded out Plain growth and is contained most and gain the name.Apocynum fibre has many excellent characteristics, soft and good luster, has silk
Gloss, the very light of fiber crops, the softness of cotton, the malleability of floss, and have pharmacological action, be once described as " wild by crudefiber crop expert Feng Yunhe etc.
The king of fiber ", is therefore 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 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, in substantially irregular kidney-shaped, lumen is less in section, and fiber longitudinally no reverses, and there are many vertical lines on surface have
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 Herba Apocyni veneti bast has certain difference with other bast-fibres.Herba Apocyni veneti bast hemicellulose level
16.31%, content of lignin 12.09%, it is above Boehmeria Caulis et Folium Lini Fructus Cannabiss, especially content of lignin is apparently higher than other fiber crops
Class, and content of cellulose only 45.74% is minimum in all bast-fibres.
Because Herba Apocyni veneti bast non-cellulose components are 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, the more other bast-fibre of apocynum degumming is increasingly difficult, 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 leading to 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, and chemical Degumming is difficult between Proper Match fibre strength, length and fineness simultaneously
Relation, 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, leads to 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 bioanalysises, 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, therefore bioanalysises have that degumming quality is unstable, efficiency is low, consumption
The problems such as duration, high cost, 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., and 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, generally require multiple repetition exploding technology, 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 that raw material carries out pretreatment, when relying on the single effect degumming of chemistry, biological or physics, processing conditionss are difficult to
Control, fibre strength is 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 to concentrate on the softening of fiber and the soft treatment of textile mostly,
Without 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 production method that becomes more meticulous 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.
Content of the invention
It is an object of the present invention to provide a kind of production method that becomes more meticulous of Herba Apocyni veneti degummed ramie, to overcome prior art
The apocynum fibre that time-consuming for Degumming method generally existing, chemical drugss usage amount is big, prepared is short, thick, hard, intensity is inclined
Low technical problem.
The present invention be employed technical scheme comprise that for achieving the above object, a kind of producer that becomes more meticulous of Herba Apocyni veneti degummed ramie
Method is it is characterised in that comprise the following steps：
The first step, the steaming and decocting remove impurity of Herba Apocyni veneti bast infiltrates activation step with organic amine
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；, to seething with excitement, steaming and decocting 0.5～1 hour under fluidized state, to carry out Herba Apocyni veneti bast remove impurity for heating cooking liquor
Process；
Then, the Herba Apocyni veneti bast through steaming and decocting remove impurity is placed in vapor tight tank, being immersed in mass percent concentration is 40%
In～60% organic amine solvent, it is continuously stirred at room temperature 5～10 hours, so that Herba Apocyni veneti bast fully infiltrates activation,
Then, by the organic amine solvent vent in tank, take out the Herba Apocyni veneti bast through infiltration activation, standby；
Described 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 of agent T, penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10 or N- ethyl pyrrolidone NEP-100 or
Multiple；
Described metal ion chelation agent is sodium tripolyphosphate, sodium hexameta phosphate, sodium pyrophosphate, sodium silicate, sodium citrate, benzene
One or more of sodium formate, polyacrylamide, sodium salicylate or tetrasodium ethylenediamine tetraacetate；
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 vapor reaches 0.5～1MPa, and pressurize 1～5 minute at this pressure；
Then, rapid pressure release sudden strain of a muscle is quick-fried, obtains disperseing the Herba Apocyni veneti bast of activation；
3rd step, beats cake dress cage step
By in the numb cage of Herba Apocyni veneti 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 rotate, pancake making machine machinery foot move up and down beat reality beat Herba Apocyni veneti bast；Meanwhile, watering duckbilled from
Up to lower continuous drip washing of 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 being loaded with Herba Apocyni veneti bast is integrally placed in glue kettle, opens liquid feed valve, makes
Into glue kettle, first inject ferrous salt solution to liquid level with high-pressure pump and do not have Herba Apocyni veneti bast；
Then, continue to keep high-pressure pump operating, so that ferrous salt solution and outside ferrous salt solution are forced to follow in glue kettle
Ring, after in holding glue kettle, ferrous salt solution is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 15～30 minutes,
Stop high-pressure pump, close liquid feed valve, open liquid valve, close liquid valve by after the ferrous salt solution emptying in glue kettle；
Then, open liquid feed valve, into glue kettle, first inject activator body lotion using high-pressure pump 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,
After in holding glue kettle, activator body lotion is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 0.5～1.2 hour, stop
High-pressure pump, close liquid feed valve, open liquid valve, closing liquid valve by 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
Open liquid feed valve, pump into alkaline degumming liquid into glue kettle, do not have a Herba Apocyni veneti bast to liquid level, heated and boiled, and
Continuously cooking 0.5～1 hour under fluidized state；
Then, empty degumming liquid, injection sulphuric acid body lotion or hydrochloric acid body lotion wash Herba Apocyni veneti bast 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, oiling, dry, obtain final product Herba Apocyni veneti degummed ramie finished product.
Be preferably, above-mentioned organic amine solvent be one of ethylenediamine, dimethylformamide or dimethyl acetylamide or
Several.
Further preferably, above-mentioned ferrous salt solution is FeSO4Solution, FeCl2Solution or (NH4)Fe(SO4)2Solution, quality
Percent 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
For 30 DEG C～50 DEG C；Bath raio is 1 10.
Further preferably, the sodium hydroxide solution that above-mentioned alkalescence degumming liquid is 0.1%～1% for mass percent concentration；
Or, the body lotion making as follows：
Add sodium hydroxide in used steaming and decocting remove impurity waste liquid, so that the mass percent of sodium hydroxide therein is dense
Degree reaches 0.1%～1% body lotion；
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 production method that becomes more meticulous of above-mentioned Herba Apocyni veneti degummed ramie is it is characterised in that obtained spreads out
The fineness of flaxen fiber finished product is 3～4.3dtex, and residual gum content is 3.68%～5.22%, and fibre strength is 4～7.8cN/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 (for 3～4.3dtex), fibre strength index good (for 4～7.8cN/dtex), fibre
Dimension quality excellent (average length is more than 35mm)；
The production method that becomes more meticulous of the Herba Apocyni veneti degummed ramie of technique scheme, in whole production process, chemical cost
Amount is little, environmental protection pressure mitigates, and technique controlling difficulty is greatly reduced；The utility consumption such as water power vapour are little, production efficiency is high, raw
Produce low cost.
For more fully understanding the technical characterstic of the present invention, show labor and be described as follows：
In technique scheme, Herba Apocyni veneti bast raw material is carried out steaming and decocting remove impurity, steaming and decocting dedoping step can remove sieve
Cloth fiber crops bast in most of hydrotrope and part hemicellulose (the part hemicellulose on Herba Apocyni veneti bast, at high temperature, can
Hydrolysis are occurred to be removed), and then reduce consumption and the consumption of subsequent chemistry reagent.
Meanwhile, in steaming and decocting dedoping step, under the infiltration, wetting action of 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, wetting action, strengthens Herba Apocyni veneti tough
The infiltration accessibility of skin, accelerates the penetrating into of organic amine in organic amine infiltration activation, accelerates organic amine infiltration activation process.
In addition, under surfactant infiltration, moistening, dispersion and emulsification, can rapidly remove Herba Apocyni veneti bast former
Original major part inorganic matters in material, especially can remove easily absorption, complexation or chelating Fe2+The impurity of ion, it is subsequently fixed to prevent
The Fe being added in catalytic oxidation stage2+Ion " inactivates ".
Furthermore, under surfactant infiltration, moistening, dispersion and emulsification, can quickly remove Herba Apocyni veneti bast raw material
In original major part oily matter, strengthen Herba Apocyni veneti bast wellability, improve follow-up directional catalyzing oxidation step in spread out
Numb bast is to Fe2+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 containing, thus the catalytic decomposition 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 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 in the presence of organic amine, in Herba Apocyni veneti bast raw material
Hydrogen bond is destroyed, and the combination of the colloid such as lignin, hemicellulose, pectin and colloid and colloid and cellulose weakens, and structure becomes
Loose, the amorphous region of cellulose increased and by swollen simultaneously), the activation processing through organic amine simultaneously, it is possible to decrease final
The rigidity of keen-witted and capable gunny products, lifted its flexibility, can textile processibility and comfort；
Meanwhile, while the short texture that Herba Apocyni veneti bast raw material becomes in the presence of organic amine solvent, after being conducive to
The entrance of vapor and aqueous water during continuous steam explosion, strengthens and subsequently dodges quick-fried effect.
In technique scheme, the Herba Apocyni veneti bast infiltrating activation processing through organic amine is carried out at steam explosion activation
Reason, in the process, the vapor of high-temperature high-pressure state and aqueous water act on Herba Apocyni veneti raw material, and raw material is filled further
Divide swelling；Then, in the presence of moment pressure release, Herba Apocyni veneti bast is made to loosen or disperse, the steam realizing Herba Apocyni veneti bast dodges
Quick-fried activation processing.
In technique scheme, beat during cake using while beat cake, while hot water spray method, live to infiltrating through organic amine
Change process and the Herba Apocyni veneti bast of the quick-fried activation processing of sudden strain of a muscle carries out buying cake, the colloid in Herba Apocyni veneti bast can be made to make in the immersion of warm water
Softened further with lower, and partly remove in the presence of mechanical force；Especially, beat during cake due to mechanical external force effect and
Warm water process acts on, and 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.
Meanwhile, in technique scheme, in beating cake dress cage step, using the warm water drip washing when pancake making machine buys cake, can be
Beat real while beat Herba Apocyni veneti bast, wash off by the metal ion chelation agent brought in steaming and decocting remove impurity in Herba Apocyni veneti bast, prevent
The Fe only being added in follow-up directional catalyzing oxidation step2+Ion " inactivates ".
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 in the presence of oxy radical and
Adsorb more Fe in the presence of organic amine infiltrates the nitrogen-containing group of the organic amine brought in activation process2+.
After adding activator, it is adsorbed with Fe2+Hemicellulose and lignin take the lead in oxidized degraded, partly oxidized degraded
Directly dissolve removal for small organic molecule, be partly 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, that is, be 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.
In technique scheme, in chemical Degumming step, degumming liquid is to pass through to add 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, originally as hot water, is re-used for chemical Degumming step and can reduce whole technical process
Energy consumption.What is more important, because steaming and decocting remove impurity waste liquid itself contains surfactant, directly utilizes to it, can avoid chemistry
The addition again of surfactant in degumming step, reduces the consumption of whole technical process chemicals, increases making of chemicals
Use efficiency.
Wherein, using organic amine infiltration activation, steam explosion activation and Fe2+Ion and hydrogen peroxide (or peracetic acid or
Carbamide peroxide solution) soak that to be oriented catalytic oxidation treatment to Herba Apocyni veneti bast be one of key problem in technology point of the present invention,
Very crucial effect is served to final apocynum fibre treatment effect.Reason is as follows：
In 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 length is 20～25mm, and 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 disperse.Traditional is de-
Gluing method is all made by the effect of chemical reagent or enzyme, successively strips down the colloid in bundle fiber from outside to inside, causes
Make degumming degree inside and outside raw material inconsistent, outer layer degumming degree is better than internal layer, lead to end article quality decline, simultaneously this process
Reaction condition is wayward, if degumming effect is acutely, fiber can be led to shorten, lose weaving use value；If degumming effect
Bad, residual gum content is higher, and fiber will be led to thick, hard, rough, is equally unfavorable for that follow-up textile process operation uses.
Therefore, to change the degumming mode successively peeling off colloid from outside to inside, with condition Proper Match sieve of milder
Relation between cloth fiber crops process of fiber intensity, fineness, length, needs the orientation that raw material is carried out with 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 plain degree of polymerization, destroy that in raw material, the component molecules such as lignin, hemicellulose are interior and intermolecular and lignin, half fibre
Hydrogen bond between dimension element and cellulosic molecule, weakens colloid and colloid and colloid and the adhesion of cellulose, increases raw material simultaneously
Swollen degree, partial removal hemicellulose and lignin, the infiltration beneficial to degumming reagent simultaneously has an effect further.Meanwhile,
Using organic amine as activating reagent, can also on the one hand act on lignin increases its water solublity, on the other hand possesses brilliant work that disappear
With material crystal degree can be reduced, increases amorphous region area, improve raw material hydrophilic, therefore, be more beneficial for reducing further
The difficulty of follow-up degumming.
What is more important, in the presence 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
The 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, because the colloids such as hemicellulose and lignin are wrapped in fibrous outer, it is thus in the half of raw material surface
Cellulose and content of lignin increase, and make more groups containing O be exposed to raw material surface, power containing O in hemicellulose and lignin
In the presence 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 organic amine infiltration activation process in, organic amine material can be brought in Herba Apocyni veneti bast raw material, in organic amine containing nitrilo
Group also can strengthen Herba Apocyni veneti bast raw material Fe2+The activity of ionic adsorption, beneficial to Fe in follow-up orientation activation process2+The suction of ion
Attached, and then be conducive to the carrying out of follow-up directional catalyzing oxidation.
In addition, the steam explosion activation processing of technique scheme, because steam explosion processes low intensity, 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 are interior and intermolecular and lignin, hemicellulose and cellulosic molecule between hydrogen bond, weaken colloid and colloid and
Colloid and the adhesion of cellulose, increase swollen degree, partial removal hemicellulose and the lignin of raw material, beneficial to follow-up simultaneously
The infiltration of chemical reagent is simultaneously had an effect further.
Meanwhile, in the steam explosion activated process of technique scheme, high temperature, the vapor of high pressure conditions and liquid
Water acts on the Herba Apocyni veneti bast raw material through organic amine infiltration activation, and raw material is carried out with abundant swollen, subsequent moment pressure release
Cheng Zhong, under the effect of class mechanical disintegration, the synergy of hydrogen bond destruction and 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, so that Herba Apocyni veneti bast raw material specific surface area is increased, follow-up Fe can be strengthened2+The absorption of ion.
Meanwhile, during steam explosion, in the presence of class acidic hydrolysises 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 fracture between cellulose, between lignin and cellulose or weaken, makes Herba Apocyni veneti raw material be loosened or disperse, makes former
While material specific surface area increases, because the colloids such as hemicellulose and lignin are wrapped in fibrous outer, it is thus in stock chart
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 group, can the more Fe of active adsorption2+Ion, enhances Herba Apocyni veneti bast raw material Fe2+Ionic adsorption
Activity, beneficial to Fe 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 dodging quick-fried activation process, the vapor of high-temperature high-pressure state and aqueous water, can be well to being difficult removal
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 separates and removes, and reduces difficulty and the intensity that follow-up directional catalyzing oxidation is processed with soda boiling, reduces 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, Herba Apocyni veneti bast raw material has obtained effectively loosening or disperseing, takes off with the chemical Degumming method of prior art and biology
Gluing method is compared, and can save and copy numb step after soda boiling degumming, reduce energy consumption and water consume.
In directional catalyzing oxidizing process, infiltrate activation processing and the Herba Apocyni veneti raw material of the quick-fried activation processing of sudden strain of a muscle through organic amine,
Due to hemicellulose and lignin Surface oxygen-containing groups increase and nitrogen-containing group introducing, in FeSO4、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 is processed, the Fe of hemicellulose and lignin absorption2+Directly add in 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 extremely strong HO of raw oxidability, the extremely strong HO of the oxidability due to producing are predominantly located at hemicellulose and lignin table
Part hemicellulose therefore can be degraded to water soluble small organic molecule and be dissolved in the water by face；Simultaneously because
HO oxidability is extremely strong, by complex structure and can be difficult to lignin side chain C-C bond fission or the generation ring-opening reaction removing, raw
Subsequent chemistry degumming is become to be more easy to the structure removing it is easy to follow-up degumming removes.HO Oxidation radius very little 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 the remaining most non-cellulosic material of removal, especially may be used
Make oxidized rear side chain C-C bond fission or occur the lignin of ring-opening reaction to occur hydrolysis to remove so that fiber enters one
Step dispersion, simultaneously cellulose disappear under alkali liquor brilliant effect, reduce degree of crystallinity, the hydrophilic of raising fiber, softening fibre.
In technique scheme, through infiltration activating pretreatment after Herba Apocyni veneti bast raw material, need not wash, directly enter
Row steam explosion pretreatment.Main cause, one is that the organic amine having neither part nor lot in priming reaction in steam explosion preprocessing process enters
One step activates to Herba Apocyni veneti bast, and two is the activation effect for effective protection organic amine to Herba Apocyni veneti bast raw material.
In technique scheme, break the Herba Apocyni veneti bast raw material after cake, need not wash, that is, be directly injected into ferrous salt solution and enter
Row is processed, and main cause is, the remaining organic amine reagent of not yet removal completely during buying cake, and former with apocynum fibre
There is the organic amine reagent of chemical reaction in material, can adsorb more Fe under the left and right of the N element that organic amine itself contains2+, increase
Strong catalytic oxidation effect.
In technique scheme, why by the Herba Apocyni veneti aoxidizing through directional catalyzing bast raw material, need not wash, that is, exist
Emptying reactant liquor after, be pumped directly into alkali liquor carry out degumming process it is therefore intended that, one is, wherein remaining undecomposed activator can
To increase degumming effect and bleaching effect in soda boiling scouring processes, two are, remaining Fe2+Degumming liquid can be carried out with coagulation take off
Color, mitigates subsequent wastewater treatment difficulty.
Certainly, correspondingly, pre- acid treatment, pre- alkali process, in advance the urine oxygen process chemical Degumming method contrast with prior art,
Before chemical Degumming, eliminate a water-washing step, reduce 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 in journey coagulation decoloration effect, the coloring matter in effluent part can be taken off.Therefore, to produced during subsequent production
Waste water decoloring intractability accordingly reduces.
Meanwhile, the chemical Degumming method ratio with 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 catalysises activator produces is made
Be there is efficiency high, polluted the significant advantage such as little with carrying out apocynum fibre degumming.
In technique scheme, pickling, then in order to neutralize the alkaline reagent of chemical Degumming, prevents alkali from entering one to cellulose
Step degraded；Oil to improve the apparent condition of fiber, increase laxity and the softness of fiber, be easy to subsequently spin.
In a word, the combination just because of above-mentioned series technique means is so that in apocynum fibre crude product alkaline boiling,
Process compared with the steaming and decocting of prior art, be all greatly decreased in terms of chemical levels, steaming and decocting required time or save, this is for having
Effect mitigates the damage to fibrous physics index for the alkaline scouring process, and reduction wastewater treatment difficulty, alleviation environmental protection pressure, raising produce effect
Rate, reduces production cost and is respectively provided with obvious positive effect.
Supplementary notes：In technique scheme, apocynum fibre after alkaline scouring is processed, remaining colloid in fiber
And pigment, removed further, thus reaching ideal flax fiber separation index and whiteness index.
In sum, the present invention, with respect to prior art, has the advantages that：
1st, degumming effect good (residual gum content is 3.68%～5.22%), the Herba Apocyni veneti degummed ramie finish fineness being obtained is thin
(for 3～4.3dtex), fibre strength index good (for 4～7.8cN/dtex), (average length is more than average fiber length length
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, production efficiency is high, production cost is greatly reduced.
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
Production 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 bast through steaming and decocting remove impurity is placed in vapor tight tank, is immersed in the second two that mass percent concentration is 40%
In amine, it is continuously stirred at room temperature 5 hours, so that Herba Apocyni veneti bast fully infiltrates activation；
Then, the ethylenediamine in tank is vented, takes out the Herba Apocyni veneti bast through infiltration activation.
Herba Apocyni veneti raw material after ethylenediamine infiltration activation is directly placed in steam explosion device, heating makes steam explosion fill
Water vapour pressure in putting is 0.8MPa, keeps this pressure 1 minute；Then open valve, rapid pressure release；
Collect the apocynum fibre spraying from steam explosion equipment, then carry out buying cake, cake gained Herba Apocyni veneti will be beaten tough
Skin and numb 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, makes FeSO using high-pressure pump4Solution inner-outer circulation 15 minutes, empties FeSO4After solution, pump into mass percent
Concentration is 0.5% hydrogen peroxide solution, after 30 DEG C of circular treatment 0.8 hour, emptying hydrogen peroxide solution, pumps into mass percent
Concentration is 0.1% sodium hydroxide solution, and boiling boils 0.5 hour.
Then, pickling is carried out at room temperature to the fiber after steaming and decocting, 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.
Fiber washing to pH value is neutrality, finally, successively after being dehydrated, oil, drying, 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 Herba Apocyni veneti degummed ramie residual gum content is 5.22%, and average fiber length is more than 35mm, and fibre strength is
7.8cN/dtex, fibre fineness is 4.3dtex.
Embodiment 2
The Herba Apocyni veneti bast places of origin of raw materials：Xinjiang
Production 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 bast through steaming and decocting remove impurity is placed in vapor tight tank, is immersed in the diformazan that mass percent concentration is 40%
In base Methanamide, it is continuously stirred at room temperature 10 hours, so that Herba Apocyni veneti bast fully infiltrates activation；
Then, the dimethylformamide in tank is vented, takes out the Herba Apocyni veneti bast through infiltration activation.By dimethyl methyl
Herba Apocyni veneti raw material after amide infiltration activation is directly placed in steam explosion device, and heating makes the vapor in steam explosion device
Pressure is 1MPa, keeps this pressure 5 minutes；Then open valve, rapid pressure release；
Collect the apocynum fibre spraying from steam explosion equipment, then carry out buying cake, cake gained Herba Apocyni veneti will be beaten tough
Skin and numb 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, makes FeCl using high-pressure pump2Solution inner-outer circulation 30 minutes, empties FeCl2After solution, pump into mass percent
Concentration is 2.5% peracetic acid soln, after 50 DEG C of circular treatment 1 hour, emptying peracetic acid soln, pumps into percent mass
Specific concentration is 0.1% sodium hydroxide solution, and boiling boils 1 hour.
Then, pickling is carried out at room temperature to the fiber after steaming and decocting, 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.
Fiber washing to pH value is neutrality, finally, successively after being dehydrated, oil, drying, 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 dodecyl sodium sulfate；
Above-mentioned metal ion chelation agent is sodium hexameta phosphate.
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 4cN/
Dtex, fibre fineness is 3dtex.
Embodiment 3
The Herba Apocyni veneti bast places of origin of raw materials：Xinjiang
Production method：Except FeSO4Solution quality percent concentration is 1%, the time of alkaline degumming liquid continuously cooking is little for 1
When, using carbamide peroxide solution substitute hydrogen peroxide, using dimethyl acetylamide replace ethylenediamine, carbamide peroxide Solutions Solution
Mass percent concentration be 1.5% outside；
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
6.3cN/dtex, fibre fineness is 4.1dtex.
It is to be noted that：
1st, above-mentioned surfactant is it is also possible that such as：Dodecyl sodium sulfate, sodium lauryl sulphate, dodecyl
Benzene sulfonic acid sodium salt, dioctyl sodium sulfosuccinate, Laurel alcohol sulfuric ester MA24F, SAS SAS60, pull open powder, quickly ooze
Agent T, penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10, N- ethyl pyrrolidone NEP-100 thoroughly；
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 it 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.
2nd, organic amine solvent can also be the mixing two-by-two or three of ethylenediamine, dimethylformamide or dimethyl acetylamide
The mixture of person.
Claims (6)
1. a kind of production method that becomes more meticulous of Herba Apocyni veneti degummed ramie is it is characterised in that comprise the following steps：
The first step, the steaming and decocting remove impurity of Herba Apocyni veneti bast infiltrates activation step with organic amine
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 seethe with excitement, steaming and decocting 0.5～1 hour under fluidized state, with carry out Herba Apocyni veneti bast remove live together
Reason；
Then, the Herba Apocyni veneti bast through steaming and decocting remove impurity is placed in vapor tight tank, be immersed in mass percent concentration be 40%～
In 60% organic amine solvent, it is continuously stirred at room temperature 5～10 hours, so that Herba Apocyni veneti bast fully infiltrates activation, so
Afterwards, by the organic amine solvent vent in tank, take out the Herba Apocyni veneti bast through infiltration activation, standby；
Described 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 of penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10 or N- ethyl pyrrolidone NEP-100；
Described metal ion chelation agent is sodium tripolyphosphate, sodium hexameta phosphate, sodium pyrophosphate, sodium silicate, sodium citrate, benzoic acid
One or more of sodium, polyacrylamide, sodium salicylate or tetrasodium ethylenediamine tetraacetate；
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 vapor reaches 0.5～1MPa, and pressurize 1～5 minute at this pressure；
Then, rapid pressure release sudden strain of a muscle is quick-fried, obtains disperseing the Herba Apocyni veneti bast of activation；
3rd step, beats cake dress cage step
By in the numb cage of Herba Apocyni veneti 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 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 continuous drip washing of 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 being loaded with Herba Apocyni veneti bast is integrally placed in glue kettle, opens liquid feed valve, using height
Press pump first injects ferrous salt solution to liquid level into 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
Hold after ferrous salt solution is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 15～30 minutes in glue kettle, stop high pressure
Pump, close liquid feed valve, open liquid valve, closing liquid valve by after the ferrous salt solution emptying in glue kettle；
Then, open liquid feed valve, into glue kettle, first inject activator body lotion to liquid level using high-pressure pump 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-
After activator body lotion is all the time with swiftly flowing state constant impingement Herba Apocyni veneti bast 0.5～1.2 hour in glue tank, stop high pressure
Pump, close liquid feed valve, open liquid valve, closing liquid valve by 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
Open liquid feed valve, pump into alkaline degumming liquid into glue kettle, do not had Herba Apocyni veneti bast, heated and boiled to liquid level, and boiling
Rise continuously cooking 0.5～1 hour under state；
Then, empty degumming liquid, injection sulphuric acid body lotion 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
By obtained apocynum fibre semi-finished product successively through being dehydrated, oiling, dry, obtain final product Herba Apocyni veneti degummed ramie finished product.
2. the production method that becomes more meticulous of Herba Apocyni veneti degummed ramie according to claim 1 is it is characterised in that described organic amine
Solvent is one or more of ethylenediamine, dimethylformamide or dimethyl acetylamide.
3. the production method that becomes more meticulous of Herba Apocyni veneti degummed ramie according to claim 1 is it is characterised in that described ferrous salt is molten
Liquid is FeSO4Solution, FeCl2Solution or (NH4)Fe(SO4)2Solution, mass percent concentration is 0.03%～1%.
4. the production method that becomes more meticulous of Herba Apocyni veneti degummed ramie according to claim 1 is 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. the production method that becomes more meticulous according to the arbitrary described Herba Apocyni veneti degummed ramie of claim 1-4 is it is characterised in that described alkali
The sodium hydroxide solution that property degumming liquid is 0.1%～1% for mass percent concentration；
Or, the body lotion making as follows：
Add sodium hydroxide 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 described sulphuric acid body lotion or hydrochloric acid body lotion is 0.1%, and bath raio is 1 20.
6. the production method that becomes more meticulous according to the arbitrary described Herba Apocyni veneti degummed ramie of claim 1-4 is it is characterised in that obtained
Herba Apocyni veneti degummed ramie finished product fineness 3～4.3dtex, residual gum content be 3.68%～5.22%, fibre strength be 4～7.8cN/
Dtex, the average length of fiber is more than 35mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107119334A (en) * | 2017-06-28 | 2017-09-01 | 梁国柱 | A kind of apocynum fibre degumming method of comprehensive utilization |
| CN107821131A (en) * | 2017-10-20 | 2018-03-23 | 东营市农业科学研究院 | A kind of beach saline land bluish dogbane implantation methods |
| WO2021237519A1 (en) * | 2020-05-27 | 2021-12-02 | 南通纺织丝绸产业技术研究院 | Method for treating flash-explosion of supercritical co2 fluid for natural fiber |
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| KR20140062642A (en) * | 2012-11-14 | 2014-05-26 | 이경종 | Degumming method of bast fiber |
| CN104264232A (en) * | 2014-08-27 | 2015-01-07 | 青岛大学 | Preparation method of functional bast fiber through degumming and modification |
| CN105256384A (en) * | 2015-10-20 | 2016-01-20 | 东华大学 | Method for oxidation degumming of ramie under weak acid condition |
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| US20040191888A1 (en) * | 2001-07-10 | 2004-09-30 | Clarke Adrian Francis K. | Degumming of bast fibres |
| CN101550607A (en) * | 2009-05-16 | 2009-10-07 | 太原理工大学 | Hemp fiber degumming boiling-off additive, preparing method and application thereof |
| KR20140062642A (en) * | 2012-11-14 | 2014-05-26 | 이경종 | Degumming method of bast fiber |
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| CN107119334A (en) * | 2017-06-28 | 2017-09-01 | 梁国柱 | A kind of apocynum fibre degumming method of comprehensive utilization |
| CN107119334B (en) * | 2017-06-28 | 2019-02-19 | 梁国柱 | A kind of apocynum fibre degumming method of comprehensive utilization |
| CN107821131A (en) * | 2017-10-20 | 2018-03-23 | 东营市农业科学研究院 | A kind of beach saline land bluish dogbane implantation methods |
| WO2021237519A1 (en) * | 2020-05-27 | 2021-12-02 | 南通纺织丝绸产业技术研究院 | Method for treating flash-explosion of supercritical co2 fluid for natural fiber |
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