CN106567138A - Refined processing method of hemp fiber - Google Patents

Refined processing method of hemp fiber Download PDF

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Publication number
CN106567138A
CN106567138A CN201610952062.1A CN201610952062A CN106567138A CN 106567138 A CN106567138 A CN 106567138A CN 201610952062 A CN201610952062 A CN 201610952062A CN 106567138 A CN106567138 A CN 106567138A
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hemp
phloem
sodium
degumming
body lotion
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CN106567138B (en
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张元明
韩光亭
徐颖
李明华
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
    • D01C1/02Treatment of vegetable material by chemical methods to obtain bast fibres

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

Abstract

The invention discloses a refined processing method of hemp fiber. The refined processing method comprises following steps: cooking and impurity removing of hemp bast; steam flash explosion activation; cake making and cage packaging; orientation catalytic oxidation; chemical degumming; and postprocessing; after steam flash explosion activation, a ferrous salt solution and an activating agent are used for orientation catalytic oxidation of lignin, pectin, and hemicelluloses; organic combination of a series of technology including steam flash explosion activation and orientation catalytic oxidation is realized, so that the refined processing method of hemp fiber is excellent in degumming effect, factors of obtained hemp fiber finished products, including fineness, length, and strength, are excellent, quality is excellent, and spinnability is excellent. In processing process, chemical consumption amount is small, environment protection pressure is low, technical control is simple, public work consumption amount such as water, electricity, and gas is low, efficiency is high, and the refined processing method is suitable for industrialized production, and is promising in market popularization prospect.

Description

A kind of fine design method of hemp
Technical field
The present invention relates to a kind of processing method of flaxen fiber, more particularly to a kind of fine design method of hemp.
Background technology
Fructus Cannabiss, also known as hemp, cold fiber crops, Urtica cannabina L. etc., another name appellation up to more than ten is planted, and have " king of natural fiber " good reputation. History records are carried, and Fructus Cannabiss originate from China, the clothing finery by made by it have moisture absorption, it is ventilative, pleasant, radiate, it is mould proof, antibacterial, anti- The several functions such as radiation, anti-ultraviolet, sound-absorbing, not only can be military but also can be civilian.And made with it for effect of antimicrobial socks, just By extensive favorable comment.Fructus Cannabiss are the natural fibers that the mankind are used for earliest fabric, there is " source, 10000 years clothing ancestrals spin in state " good reputation, its kind Plant history at least more than 8000 year.
Because Fructus Cannabiss contain 17.27% hemicellulose, 5.99% pectin, 6.07% lignin, it is being applied to spin Knit needs to carry out degumming process before processing.Used as one important procedure in hemp preliminary working, degumming quality is fine or not, directly for degumming Connect and have influence on the follow-up textile process of hemp and the properties of end article.
Chemical degumming law is the main method that at present hemp fiber degumming industry both at home and abroad is adopted, and can be subdivided into by technique High Temperature High Pressure kiering and the big class of normal temperature and pressure kiering two.Wherein, the advantage of High Temperature High Pressure kiering is that degumming speed is fast, and colloid is gone Except many (cull is few), degummed ramie quality is preferable.Have the disadvantage, fiber row yielding is relatively low, made fibre length is partially short.
The advantage of normal temperature and pressure kiering is, fiber row yielding is high, made by fibre length it is longer.Have the disadvantage, degumming speed Slowly, colloid removes less (cull is more), and degummed ramie fibre separation index is poor.
And, either High Temperature High Pressure degumming or normal temperature and pressure degumming, it is big to there is chemical reagent usage amount, not only into This height, and serious to fibre damage, and waste water is difficult to process, environmental pollution is serious.
Also there is the more research about hemp biological degumming method to report in recent years, it is main including hemp biological degumming Including two methods of microbial degumming and enzyme degumming.Although through years of researches, up to the present, domestic and international hemp Biological degumming method is simultaneously immature, only rests on the test production phase.It is believed that being primarily due to hemp gum components ten Divide complexity, need corresponding complexity enzyme system collective effect, and bacterial strain often only has one or more correlations in nature Enzyme, or lack Crucial degumming enzyme, therefore need the effect of composite flora to reduce Plant fiber's colloid, reach the purpose of degumming. Degumming strain enzymatic productivity is low, strain Crucial degumming enzyme vigor is not high or the enzyme system of secretion is complete, degumming effect is unstable etc. makes Antibacterial degumming process does not reach the requirement of bast fibre spinning.Simultaneously as Fructus Cannabiss internal component is complicated, compact structure, enzyme is difficult to fully to Its degraded, thus bioanalysises there are problems that degumming quality is unstable, efficiency is low, time-consuming, being required for of major part Learn method for degumming to make up the congenital defect on its degumming tech.
Physical Degumming method include ultrasonic Treatment method, microwave treatment method and steam explosion etc., wherein, study it is the most general It is steam explosion technology all over be.But, the steam explosion treatment temperature that relevant institute is used is high, pressure is big;Particularly, it is past Toward multiple repetition exploding technology is needed, inevitably, hemp strength damage and fiber length loss will be caused.
In a word, in prior art, in the case where pretreatment is not carried out to Fructus Cannabiss raw material, by it is single it is chemical, During biological or physics effect degumming, processing conditionss are difficult to control to, and the relation between fibre strength, length, fineness is difficult to close Reason control, has a strong impact on Fructus Cannabiss product quality.
In order to improve research of hemp fiber features, promote its effectively utilizes, both at home and abroad to Fructus Cannabiss on the basis of traditional Degumming method Fiber fine techniques have also carried out a few thing, but are mostly the soft treatments of the softening and product for concentrating on hemp, and The problem that becomes more meticulous of hemp itself is not solved, this quality and added value obviously to hemp products is lifted and had little significance.
The hemp fine design processing method of low damage, is the key for lifting hemp value, is represented Industry developing direction.
The content of the invention
It is an object of the present invention to provide a kind of process conditions are gentle, degumming effect is good, in scouring processes fibre damage it is little, And the fine design method of environmental friendly hemp.
The technical scheme that adopted for achieving the above object of the present invention is, a kind of fine design method of hemp, Characterized in that, comprising the following steps:
The first step, the steaming and decocting removal step of hemp phloem
Hemp phloem is placed in rotary spherical digester, digester or cooker, injection cooking liquor by hemp phloem until be immersed in steaming Under boil liquid face;Heating cooking liquor is to boiling, steaming and decocting 0.5~1 hour under fluidized state, to carry out hemp phloem remove impurity process;
Then, the hemp phloem 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%;
The 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 powder, rapid osmotic One kind or many in agent T, penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10, N- ethyl pyrrolidone NEP-100 Kind;
The 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, tetrasodium ethylenediamine tetraacetate;
Second step, dodges quick-fried activation process step
The hemp phloem after remove impurity is processed is placed in steam explosion device, is passed through steam, until steam explosion dress The pressure for putting 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 hemp phloem of activation;
3rd step, beats cake dress cage step
By in the numb cage of hemp phloem feeding of resulting dispersion activation, cake is beaten using pancake making machine;During feeding, numb cage is with 3 ~5 revs/min of speed does not stop rotation, and pancake making machine machinery foot moves up and down to beat and beats hemp phloem in fact;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 hemp phloem is integrally placed in glue kettle, opens liquid feed valve, is used High-pressure pump first injects ferrous salt solution into glue kettle and did not had hemp phloem to liquid level;
Then, continue to keep high-pressure pump operating, so that ferrous salt solution is forced to follow with outside ferrous salt solution in glue kettle Ring, keeps ferrous salt solution in glue kettle all the time with swiftly flowing state constant impingement hemp phloem, after 15~30 minutes, to stop High-pressure pump, closing liquid feed valve, opening liquid valve, will close liquid valve after the ferrous salt solution emptying in glue kettle;
Then, liquid feed valve is opened, first activator body lotion to liquid level is injected into glue kettle using high-pressure pump and was not had Fructus Cannabiss 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 Activator body lotion is held in glue kettle all the time with swiftly flowing state constant impingement hemp phloem, after 1~2 hour, 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;
The activator is H2O2, peracetic acid or carbamide peroxide solution;
5th step, chemical Degumming step
Alkaline degumming liquid is pumped into into glue kettle, did not had hemp phloem, heated and boiled to liquid level, and connected under fluidized state Continuous steaming and decocting 0.5~2 hour;
Then, liquid valve is opened, after degumming liquid emptying liquid valve is closed;
Then, liquid feed valve is opened, sulphuric acid body lotion or hydrochloric acid body lotion is injected into glue kettle, hemp phloem is washed to pH value ≤7;Clear water rinsed clean repeatedly is reused, hemp semi-finished product are obtained;
6th step, post-processing step
Resulting hemp semi-finished product successively Jing are dehydrated, are oiled, are dried, hemp finished product is obtained final product.
Preferably, above-mentioned ferrous salt solution is FeSO4Solution, FeCl2Solution or (NH4)Fe(SO4)2Solution, quality percentage Specific 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, 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 body lotion or hydrochloric acid body lotion is 0.1%, and bath raio is 1:20.
Further preferably, the fine design method of above-mentioned hemp, it is characterised in that obtained hemp 2.2~the 3.5dtex of fineness of finished product, residual gum content is 2.44~3.82%, and fibre strength is 2.7~3.3cN/dtex, fiber Average length is more than 30mm.
What above-mentioned technical proposal was directly brought has the technical effect that, degumming effect good (residual gum content is 2.44~3.82%), institute Obtained hemp finish fineness thin (being 2.2~3.5dtex), fibre strength index good (being 2.7~3.3cN/dtex) are fine Dimension quality excellent (average length is more than 30mm);
The fine design method of the hemp of above-mentioned technical proposal, in whole production process, chemical cost amount is 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, produce into This is low.
To more fully understand the technical characterstic of the present invention, show labor and be described as follows:
In above-mentioned technical proposal, hemp phloem raw material is carried out into steaming and decocting remove impurity, Fructus Cannabiss are can remove in steaming and decocting dedoping step (the part hemicellulose on hemp phloem at high temperature, water to most of hydrotrope and part hemicellulose in bast can occur Solution is reacted and is removed), and then reduce consumption and the consumption of subsequent chemistry reagent.
Meanwhile, in steaming and decocting dedoping step, under the infiltration, wetting action in high temperature and surfactant, Fructus Cannabiss can be softened tough The sclerderm of epidermis 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 hemp phloem raw material are rapidly removed, easily absorption, complexation or chelating Fe is especially can remove2+From The impurity of son, prevents the Fe added in follow-up directional catalyzing oxidation step2+Ion " inactivation ".
In addition, under surfactant infiltration, moistening, dispersion and emulsification, can quickly remove in hemp phloem raw material Original most of oily matter, strengthens the wellability of hemp phloem, improves hemp phloem in follow-up directional catalyzing oxidation step To Fe2+The adsorption efficiency of ion.
Meanwhile, under the chelation of metal ion chelation agent, steaming and decocting removal step can be removed effectively contained by hemp phloem Some metal cation components, so as to be prevented effectively from the cartalytic decomposition effect of the activator that these metal cation components are likely to result in. That is, the effect of follow-up directional catalyzing oxidation is better ensured that.
In above-mentioned technical proposal, the hemp phloem after steaming and decocting remove impurity is processed is carried out into steam explosion activation processing, During this, the vapor and aqueous water of high-temperature high-pressure state act on Fructus Cannabiss raw material, raw material are carried out fully swelling;Then, In the presence of moment pressure release, hemp phloem is loosened or is disperseed, realize the activation processing of hemp phloem.
In above-mentioned technical proposal, the water-washing step of quick-fried activation process step is dodged, can directly remove glue during steam explosion Poly- macromole colloid drops in the small molecule and part that matter is degraded generated, and reduces the consumption of subsequent processing steps chemicals;More Importantly, water-washing step can effectively remove the metal ion chelation agent for bringing hemp phloem in hemp phloem digestion process into, Prevent the Fe in directional catalyzing oxidation step2+Ion " inactivation ".
In above-mentioned technical proposal, beat during cake using while beat cake, while hot water spray method, to the Jing quick-fried activation processing of sudden strain of a muscle Hemp phloem carry out buying cake, the colloid in hemp phloem can be made further to soften under the action of soaking of warm water, and in machinery Partly remove in the presence of power;Especially, beat during cake due to mechanical external force effect and warm water process effect, can effectively remove Subsequent handling is difficult to the part hemp phloem top layer sclerderm for removing, and then following process process intensity can be greatly reduced, 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 on scattered hemp phloem surface, pectin and lignin adsorb Fe in the presence of oxy radical2+
After adding activator, Fe is adsorbed with2+Hemicellulose, pectin and lignin take the lead in being oxidized degraded, partly by oxygen Change is degraded to small organic molecule and directly dissolves removal, is partly oxidized to the material that subsequent chemistry degumming is more easy to remove.
In directional catalyzing oxidation step, adsorb Fe2+Hemp phloem, without washing, that is, be placed directly within containing activator In solution, it is therefore an objective to protect Fe2+Directional catalyzing activator decomposes, and then oxidative lignin, hemicellulose and pectin, strengthens catalysis Oxidation effectiveness.
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, being re-used for chemical Degumming step 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 for chemicals Use efficiency.
Wherein, using steam explosion activation and Fe2+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 hemp phloem, at final hemp Reason effect serves very crucial effect.Reason is as follows:
In hemp phloem portion, hemp cellulose fiber is under the cementation of the colloids such as pectin, hemicellulose and lignin Bunchy (technique) fiber, wherein ultimate fibre length be 15~25mm, diameter then be 15~17 μm, colloid (pectin, hemicellulose, Lignin etc.) be connected with each other by hydrogen bond, covalent bond, van der Waals interaction with cellulose, these gum dispersions in the fibre between Or be enclosed in outside fiber, define 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, from outside to inside successively strips down the colloid in bundle fiber, is caused Degumming degree is inconsistent inside and outside raw material, and outer layer degumming degree is better than internal layer, causes end article quality decline, while this process is anti- Answer condition wayward, if degumming effect is violent, fiber can be caused to shorten, lose weaving use value;If degumming effect is not Good, 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, it is big with the condition Proper Match of milder to change the degumming mode for successively peeling off colloid from outside to inside Numb 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 hemp bulk composition cellulosic degree of polymerization, the component molecules such as lignin, hemicellulose, pectin in destruction raw material Hydrogen bond between interior and intermolecular and lignin, hemicellulose, pectin and cellulosic molecule, reduction colloid and colloid and colloid With the adhesion of cellulose, while increase raw material swollen degree, partial removal hemicellulose, pectin and lignin, after being beneficial to The infiltration of continuous chemical reagent 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 Fructus Cannabiss raw material, and abundant swollen is carried out to raw material, in subsequent moment pressure leak process, in the effect of class mechanical disintegration, hydrogen Under key destruction and the synergy of structural rearrangement, between hemicellulose and hemicellulose, hemicellulose and lignin it Between, between hemicellulose and cellulose, between lignin and cellulose, between pectin and pectin, between pectin and hemicellulose, Connection fracture or decrease between pectin and lignin, between pectin and cellulose, raw material is loosened or is disperseed, and makes Fructus Cannabiss tough Skin raw material specific surface area increases, and can strengthen follow-up Fe2+The absorption of ion.Meanwhile, during steam explosion, in class acidic hydrolysises And in the presence of thermal degradation, remove can part hemicellulose and pectin degrading, reduce following process and process intensity and chemistry Reagent dosage.
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 Between cellulose, between lignin and cellulose, between pectin and pectin, between pectin and hemicellulose, pectin and lignin Between, connection between pectin and cellulose fracture or weaken, Fructus Cannabiss raw material is loosened or is disperseed, make raw material specific surface area While increase, because the colloids such as hemicellulose, pectin and lignin are wrapped in fibrous outer, the half of raw material surface is thus in Cellulose, pectin and content of lignin increase, and make more groups containing O be exposed to raw material surface, in hemicellulose, pectin and wooden In the presence of plain electron-donating group containing O, can the more Fe of active adsorption2+Ion, enhances hemp phloem 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 quick-fried activation process is dodged, the vapor and aqueous water of high-temperature high-pressure state can well to being difficult to remove Hemp phloem crust carry out effective swollen, in subsequent moment pressure leak process class mechanical disintegration effect under, by itself and Fructus Cannabiss Tough endo-endothelial layer is separated and removed, and reduces difficulty and intensity that follow-up directional catalyzing oxidation and soda boiling are processed, reduces subsequent chemistry examination The usage amount of agent.
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, hemp phloem raw material has been obtained effectively loosening or disperseed, the chemical Degumming method and biological degumming with prior art Method is compared, and can save copy numb step after soda boiling degumming, reduce energy consumption and water consume.
In directional catalyzing oxidizing process, Jing dodges the Fructus Cannabiss raw material of quick-fried activation processing, due to hemicellulose, pectin and wooden Plain Surface oxygen-containing groups increase, in FeSO4、FeCl2Or (NH4)Fe(SO4)2Under the immersion of solution, Fructus Cannabiss raw material surface is a large amount of Absorption Fe2+, then in hydrogen peroxide or peracetic acid or carbamide peroxide solution are processed, hemicellulose, pectin and lignin are inhaled Attached Fe2+In the H that hemicellulose, pectin and lignin surface catalysis directly add2O2Peracetic acid or carbamide peroxide it is molten The H that liquid hydrolysis is generated2O2Decompose, in acid condition, Fe2+Catalysis H2O2Decompose and produce the extremely strong HO of oxidability, due to producing The extremely strong HO of raw oxidability is predominantly located at hemicellulose, pectin and lignin surface, therefore can be by part hemicellulose Water soluble small organic molecule is degraded to pectin and be dissolved in the water;Simultaneously because HO oxidabilities are extremely strong, can By complex structure and the lignin side chain C-C bond fissions that are difficult to remove or there is ring-opening reaction, generate subsequent chemistry degumming and be more easy to The structure of removal, it is easy to which follow-up degumming is removed.While HO Oxidation radius very littles, and because cellulose is wrapped in half fiber In element, pectin and lignin, 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 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 hemp phloem raw material aoxidized through directional catalyzing, without the need for washing, i.e., in row After empty reactant liquor, being pumped directly into alkali liquor carries out degumming process, it is therefore intended that, one is, wherein remaining, undecomposed activator can be with Increase the degumming effect and bleaching effect in soda boiling scouring processes, two are, remaining Fe2+Coagulation decoloration can be carried out to degumming liquid, Mitigate subsequent wastewater treatment difficulty.
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, reduce water consume.
In addition, compared with existing biological, chemical Degumming technology, this technology is due to remaining Fe2+Ion is in chemical Degumming mistake Act on coagulation decoloration in journey, the coloring matter in effluent part can be taken off.Therefore, to produced during subsequent production Waste water decoloring intractability is accordingly reduced.
Meanwhile, the chemical Degumming method ratio with prior art, above-mentioned technical proposal 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 is produced is made With hemp fiber degumming is carried out there is efficiency high, the significant advantage such as little is polluted.
In above-mentioned technical proposal, pickling then in order to neutralize the alkaline reagent of chemical Degumming, prevents alkali from entering one to cellulose Step degraded;The apparent condition for improving fiber is oiled, increases 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 hemp crude product alkaline boiling, compared with The steaming and decocting of prior art is processed, and aspect is greatly decreased or saves the time required to chemical levels, steaming and decocting, and this is for effective Mitigate damage of the alkaline scouring process to fibrous physics index, reduce wastewater treatment difficulty, alleviate environmental protection pressure, improve production effect Rate, reduces production cost and is respectively provided with obvious positive effect.
Supplementary notes:In above-mentioned technical proposal, the hemp after alkaline scouring process, in fiber remaining colloid and Pigment, is further removed, so as to reach ideal flax fiber separation index and whiteness index.
In sum, the present invention has 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 2.44~3.82%), obtained Hemp finish fineness thin (being 2.2~3.5dtex), fibre strength index good (being 2.7~3.3cN/dtex), fiber put down Equal length length (average length is more than 30mm), 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 hemp phloem places of origin of raw materials:Yunnan
Processing method is as follows:
Hemp phloem is placed in rotary spherical digester or digester or cooker, in being immersed in cooking liquor, fluidized state is heated to, is steamed Boil 0.5 hour, carry out hemp phloem remove impurity.
Fructus Cannabiss raw material after steaming and decocting remove impurity is directly placed in steam explosion device, heating makes the water in steam explosion device Steam pressure is 1.0MPa, keeps this pressure 1 minute;Then valve, rapid pressure release are opened.
Collect from steam explosion equipment spray hemp, then carry out beat cake, will beat cake gained hemp phloem with Numb cage is together placed in glue kettle, pumps into the FeSO that mass percent concentration is 0.05%4Solution, to not having hemp phloem, Under room temperature, FeSO is made using high-pressure pump4Solution inner-outer circulation 15 minutes, empties FeSO4After solution, mass percent concentration is pumped into For 0.5% hydrogen peroxide solution, in 30 DEG C of circular treatment 1 hour, after emptying hydrogen peroxide solution, pumping into mass percent concentration was 0.1% sodium hydroxide solution, boiling boils 1 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 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 hemp finished product.
Above-mentioned cooking liquor is the mixed aqueous solution of surfactant and metal ion chelation agent, wherein, surfactant Mass percent concentration is 0.1%, and the mass percent concentration of metal ion chelation agent is 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 hemp residual gum content is 3.82%, and average fiber length is more than 30mm, and fibre strength is 3.3cN/ Dtex, fibre fineness is 3.5dtex.
Embodiment 2
The hemp phloem places of origin of raw materials:Yunnan
Processing method is as follows:
Hemp phloem is placed in rotary spherical digester or digester or cooker, in being immersed in cooking liquor, fluidized state is heated to, is steamed Boil 0.5 hour, carry out hemp phloem remove impurity.
Fructus Cannabiss raw material after steaming and decocting remove impurity is directly placed in steam explosion device, heating makes the water in steam explosion device Steam pressure is 1.5MPa, keeps this pressure 5 minutes;Then valve, rapid pressure release are opened.
Collect from steam explosion equipment spray hemp, then carry out beat cake, will beat cake gained hemp phloem with Numb cage is together placed in glue kettle, pumps into the FeCl that mass percent concentration is 0.1%2Solution, to not having hemp phloem, in room Under temperature, FeCl is made using high-pressure pump2Solution inner-outer circulation 30 minutes, empties FeCl2After solution, pumping into mass percent concentration is 2.5% peracetic acid soln, in 50 DEG C of circular treatment 1 hour, after emptying peracetic acid soln, pumps into mass percent concentration For 0.1% sodium hydroxide solution, boil and boil 0.5 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.
It is neutrality by fiber washing to pH value, finally, successively Jing after being dehydrated, oil, dry, obtains final product hemp finished product.
Above-mentioned cooking liquor is the mixed aqueous solution of surfactant and metal ion chelation agent, wherein, surfactant Mass percent concentration is 2%, and the mass percent concentration of metal ion chelation agent is 0.3%;
Above-mentioned surfactant is sulfated castor oil;
Above-mentioned metal ion chelation agent is sodium tripolyphosphate.
Examination and test of products testing result:
Obtained hemp residual gum content is 2.44%, and average fiber length is more than 30mm, and fibre strength is 2.7cN/ Dtex, fibre fineness is 2.2dtex.
Embodiment 3
The hemp phloem places of origin of raw materials:Yunnan
Processing method:Except FeSO4Solution 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 hemp residual gum content is 3.15%, and average fiber length is more than 30mm, and fibre strength is 3.02cN/ Dtex, fibre fineness is 2.9dtex.
Embodiment 4
Except the mass percent concentration of surfactant is 1.2%, the mass percent concentration of metal ion chelation agent is 0.45%;Surfactant is outside the sulfated castor oil and dodecyl sodium sulfate mixture such as (quality);
Remaining, with embodiment 1.
Examination and test of products testing result:
Obtained hemp residual gum content is 2.52%, and average fiber length is more than 30mm, and fibre strength is 2.8cN/ Dtex, fibre fineness is 2.4dtex.
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. a kind of fine design method of hemp, it is characterised in that comprise the following steps:
The first step, the steaming and decocting removal step of hemp phloem
Hemp phloem is placed in rotary spherical digester, digester or cooker, injection cooking liquor by hemp phloem until be immersed in cooking liquor Under face;Heating cooking liquor is to boiling, steaming and decocting 0.5~1 hour under fluidized state, to carry out hemp phloem remove impurity process;
Then, the hemp phloem 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%;
The 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 powder, fast penetrant T, One or more in penetrating agent JFC, paregal O, alkylphenol polyoxyethylene TX-10, N- ethyl pyrrolidone NEP-100;
The 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, tetrasodium ethylenediamine tetraacetate;
Second step, dodges quick-fried activation process step
The hemp phloem after remove impurity is processed is placed in steam explosion device, is passed through steam, until in steam explosion 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 hemp phloem of activation;
3rd step, beats cake dress cage step
By in the numb cage of hemp phloem feeding of resulting dispersion activation, cake is beaten using pancake making machine;During feeding, 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 hemp phloem;Meanwhile, watering duckbilled is from upper 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 hemp phloem is integrally placed in glue kettle, liquid feed valve is opened, using high pressure Pump first injects ferrous salt solution into glue kettle and did not had hemp phloem to liquid level;
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 ferrous salt solution in glue kettle and, all the time with swiftly flowing state constant impingement hemp phloem, after 15~30 minutes, stop high pressure Pump, closing liquid feed valve, opening liquid valve, will close liquid valve after the ferrous salt solution emptying in glue kettle;
Then, liquid feed valve is opened, first activator body lotion is injected into glue kettle using high-pressure pump and was not had hemp phloem to liquid level;So Afterwards, continue to keep high-pressure pump operating, so that activator body lotion and external activator body lotion forced circulation in glue kettle, keep degumming Activator body lotion is all the time with swiftly flowing state constant impingement hemp phloem in tank, after 1~2 hour, stop high-pressure pump, close into Liquid valve, opening liquid valve, will close liquid valve after the activator body lotion emptying in glue kettle;
The activator is H2O2, peracetic acid or carbamide peroxide solution;
5th step, chemical Degumming step
Alkaline degumming liquid is pumped into into glue kettle, did not had hemp phloem, heated and boiled, and the continuous steaming under fluidized state to liquid level Boil 0.5~2 hour;
Then, liquid valve is opened, after degumming liquid emptying liquid valve is closed;
Then, liquid feed valve is opened, sulphuric acid body lotion or hydrochloric acid body lotion is injected into glue kettle, hemp phloem is washed to pH value≤7; Clear water rinsed clean repeatedly is reused, hemp semi-finished product are obtained;
6th step, post-processing step
Resulting hemp semi-finished product successively Jing are dehydrated, are oiled, are dried, hemp finished product is obtained final product.
2. the fine design method of hemp according to claim 1, it is characterised in that the ferrous salt solution is FeSO4Solution, FeCl2Solution or (NH4)Fe(SO4)2Solution, mass percent concentration is 0.03%~1%.
3. the fine design method of hemp according to claim 1, it is characterised in that the activator body lotion Mass percent concentration 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.
4. according to the fine design method of the arbitrary described hemp of claim 1-3, it is characterised in that the alkalescence is de- Glue 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. according to the fine design method of the arbitrary described hemp of claim 1-3, it is characterised in that obtained is big The fineness of flaxen fiber finished product is 2.2~3.5dtex, and residual gum content is 2.44~3.82%, and fibre strength is 2.7~3.3cN/ Dtex, the average length of fiber is more than 30mm.
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CN113445170A (en) * 2021-07-20 2021-09-28 襄樊富仕纺织服饰有限公司 Preparation process of high-count hemp blended cotton yarn
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CN106868862A (en) * 2017-03-21 2017-06-20 张辰龙 A kind of preparation method of degree of spinning antistatic hemp high
CN107385523A (en) * 2017-07-19 2017-11-24 苏州凯邦生物技术有限公司 A kind of biological enzyme jute fiber degumming agent
US11535954B2 (en) 2017-10-13 2022-12-27 Robert Czinner System, controller, and method for decortication processing
CN111386364A (en) * 2017-10-13 2020-07-07 罗伯特·钦纳 System, controller and method for skinning process
CN111386364B (en) * 2017-10-13 2023-02-21 罗伯特·钦纳 Controller and method for a skinning process
CN108070955A (en) * 2017-11-06 2018-05-25 江阴延利汽车饰件股份有限公司 A kind of preparation process and production system of light-high-strength linen fiber composite plates
WO2019124251A1 (en) * 2017-12-18 2019-06-27 日本製紙株式会社 Chemically modified cellulose and cellulose nanofiber, and method for producing same
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JP7233380B2 (en) 2017-12-18 2023-03-06 日本製紙株式会社 Chemically modified cellulose and cellulose nanofibers and method for producing the same
CN112616316A (en) * 2018-04-09 2021-04-06 复兴纤维有限责任公司 Degumming and scouring of bast materials for textile and pulp quality fiber production
CN109231412A (en) * 2018-10-25 2019-01-18 西南交通大学 A kind of method that ferrous ion activation Peracetic acid removes Diclofenac in water removal
US12018404B2 (en) 2019-07-16 2024-06-25 Robert Czinner System, controller, and method for decortication processing
CN113445170A (en) * 2021-07-20 2021-09-28 襄樊富仕纺织服饰有限公司 Preparation process of high-count hemp blended cotton yarn
CN114150521A (en) * 2021-12-03 2022-03-08 太原理工大学 Preparation method of hemp-based lyocell fiber pulp

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