CN106400129A - Method for efficiently degumming hemp by means of peroxidating at low temperatures under low-emission conditions - Google Patents

Method for efficiently degumming hemp by means of peroxidating at low temperatures under low-emission conditions Download PDF

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Publication number
CN106400129A
CN106400129A CN201610966640.7A CN201610966640A CN106400129A CN 106400129 A CN106400129 A CN 106400129A CN 201610966640 A CN201610966640 A CN 201610966640A CN 106400129 A CN106400129 A CN 106400129A
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degumming
peroxidating
low temperature
emission
low
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CN106400129B (en
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蒋秋冉
葛建东
陈思
邱夷平
韦峻峰
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Donghua University
National Dong Hwa University
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Donghua 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 relates to a method for efficiently degumming hemp by means of peroxidating at the low temperatures under low-emission conditions. The method includes mixing alkali metal peroxide, amide substances and water with one another to obtain degumming treating fluid; carrying out degumming treatment on to-be-degummed hemp materials by the aid of the degumming treating fluid in wetting, padding or spraying modes under certain treatment conditions; carrying out first-pass cleaning on materials obtained by means of degumming treatment by the aid of the treating fluid in environments at the temperatures ranging from 5 DEG C to -20 DEG C, then cleaning the materials until the materials are neutral and drying the materials. The treatment conditions include that the to-be-degummed hemp materials are treated by 1-10 passes under the conditions of the temperatures ranging from 5 DEG C to -80 DEG C and are treated for 10s-30s in each pass. The method has the advantages that the method is high in efficiency and includes simple processes; the treating fluid can be reused, accordingly, the method is low in energy consumption, water consumption, production cost and sewage discharge, degumming byproducts can be timely collected, and transformation of the hemp spinning industry to the low-carbon environment-friendly industry can be promoted.

Description

A kind of high-efficiency low-emission low temperature peroxidating retting method
Technical field
The invention belongs to the Degumming method field of numb material, particularly to a kind of high-efficiency low-emission low temperature peroxidating retting side Method.
Background technology
China is world Fructus Cannabiss, Boehmeria, flax production big country, and its labor productivity position is at the forefront in the world.China in 2011 Caulis et Folium Lini, Boehmeria, Fructus Cannabis specific yield are respectively 3856,1700,2629 kg/ha, far above world average.By 2012 Year, China has scale above flax spinning enterprise 282, completes 430.74 hundred million yuan of total industrial output value.
The maximum step of the most time-consuming in flaxen fiber production technology, cost source, pollution is degumming, and this step has begun to restrict The use of flaxen fiber and development.The most frequently used Degumming method is chemical Degumming, and also known as two cooking methods, the method flow process is very loaded down with trivial details, Water consumption is big, time-consuming, about 6 hours (pickling 2h, boils 1.5h, and two boil 2.5h).Five sodium, surfactant, non-acidleach preparation etc. The development of New-type adjuvant improves the degumming efficiency of fiber crops, takes 90~150min, but still needs to chemicals High Temperature High Pressure kiering, Mass loss to flaxen fiber is big, and can produce the alkaline waste water that a large amount of COD contents are high, colourity is high, causes environmental pollution.With ramie As a example fiber crops, often produce one ton of degummed ramie and produce about 60m3Waste water, the degumming waste water amount that year discharges reaches 3,000,000 tons about, and COD discharges About 7500 tons of amount.With scientific and technical development, Recent study worker attempts enzyme and the introducing retting works such as microorganism Skill, and obtain certain progress.Wherein chemistry, enzyme combination degumming method can reduce kiering number of times, save time-consuming (about three hours:1hization Learn degumming, 2h enzyme degumming) effort scutching operation, reduce flaxen fiber the extent of damage, but due to used degumming enzyme effect Single, and gum components complex structure in fiber crops, residual gum content is not up to standard, and working condition has high demands, and production technology is difficult to grasp and sets Standby input is big, and production cost is high, also cannot widely use in industrial conditions at present, therefore be difficult to promote.In addition, it is chemical, biological Combination degumming method, microbial treatments time length (24h microbial degumming, 2h chemical Degumming), though having certain feasibility, it takes off After glue, fiber quality is poor.It would therefore be highly desirable to the high new retting of a kind of high efficiency of exploitation, low stain, low cost, fiber quality Technology.
Content of the invention
The technical problem to be solved is to provide a kind of high-efficiency low-emission low temperature peroxidating retting method, the method Improve the efficiency of degumming step, reduce the blowdown of degumming step.
Degumming method efficiency high of the present invention, process is simple, treatment fluid can be recycled, energy consumption water consume is little, produce into This is low, quantity of wastewater effluent is few, and degumming by-product is collected in time, can promote flax spinning industry to low-carbon environment-friendly industrial repositioning.
A kind of high-efficiency low-emission low temperature peroxidating retting method of the present invention, including:
(1) by alkali-metal peroxide, amide substance and water mix, and obtain degumming process liquid;Wherein, degumming process liquid Middle alkali-metal peroxide content be 0.5wt.%~20.0wt.%, amide substance content be 0.5wt.%~ 20.0wt.%, balance of water;
(2) will treat that degumming process liquid in step (1) for the degumming numb material carries out degumming process;Wherein, the side of process Formula is infiltration, pads or spray, and the condition of process is:Process 1~10 road under conditions of 5~-80 DEG C, per pass 10s~ 30min;
(3) degumming process in step (2) is obtained under 5~-20 DEG C of environment using the treatment fluid obtaining in step (1) Material carries out just road cleaning, and then cleaning (washing or weak acid cooperation washing), to neutral, be dried, obtain through high-efficiency low-emission low temperature The numb material of peroxidating degumming.
In described step (1), alkali-metal peroxide is at least one in potassium peroxide, lithium peroxide and sodium peroxide.
In described step (1), amide substance is in carbamide, thiourea, acetamide, caprolactam and tetraethylammonium chloride At least one.
Treat in described step (2) that degumming numb material is Boehmeria, Fructus Cannabis, Caulis et Folium Lini, the raw ramie of Folium Agaves Sisalanae, Corchorus olitorius L. or Herba Apocyni veneti, fiber crops Fibre bundle or the flaxen fiber through preliminary degumming process.
In described step (2), the processing mode of infiltration is:Reach treating that degumming numb material immerses at the degumming for the treatment of temperature In reason liquid, cooperative mechanical effect simultaneously is processed, and process sloughs treatment fluid through roll after terminating.
The processing mode padded in described step (2) is:Degumming numb material will be treated through degumming process liquid, in treatment conditions Under padded, after padding cooperation mild mechanical effect process.
In described step (2), the processing mode of spray is:Degumming process liquid is sprayed in treating in degumming numb material, is processing Under the conditions of carry out degumming, in processing procedure cooperation mild mechanical effect process.
Described mechanism is beaten for machinery, mechanical oscillation or mechanical roll compacting.
In described step (2), dry condition is:It is dried under 10~105 DEG C of normal pressures or vacuum environment.
The recovery of described treatment fluid and regeneration:Used treatment fluid, through being warming up to 10~50 DEG C, precipitates and filters and remove The solvent components separating out, recycle process fluids can recycle again.
Treat in the present invention that degumming numb material is low in the aqueous solution treatment fluid of alkali-metal peroxide and amide substance After temperature is processed, part pectin, hemicellulose, lignin, waxiness and moieties amount less cellulose (molecular weight in material Less than 30 × 104) liquid to be treated high-efficiency dissolution and depart from, the larger cellulose fibre part of molecular weight remains, its part Crystallization plot structure is converted to noncrystalline domain, so that the final fibre whiteness obtaining, flexibility and stainability improve.Dissolve Glue, hemicellulose, lignin, waxiness and the less cellulose of moieties amount coming separates out after processing liquid temp rising, Can be collected to used for other purposes through filtration, the treatment fluid after purification can be continuing with.
Beneficial effect
(1) the degumming process liquid system in the present invention has Selective dissolution, for relatively low the becoming of degree of crystallinity and molecular weight Point there is high-efficiency dissolution ability, but the dissolubility of the cellulose components higher to degree of crystallinity and molecular weight is weaker, therefore can be Under conditions of avoiding giving fibrous body damage, by adjusting treatment conditions, controlled removing is carried out to degumming main component;
(2) the K cryogenic treatment principle in the present invention avoids hydrolysis, but directly dissolves, not only during the process of technique Between shorter, thus shortening the degumming tech time, save production cost;Meanwhile, dissolved material can process liquid temp lifting After separate out and be collected, thus the dissolved material with macromolecular structure can be further used for other application;
(3) present invention passes through the Oxidation of low temp alkali metal peroxide and amide substance water solution system, accelerates Degumming, simultaneously can also be to fiber bleached and give its certain biocidal property;
(4) process in the present invention can open the crystal region of cellulose system to a certain extent, and crystal region is converted to Amorphous area, thus improve flexibility and the stainability energy of fiber;
(6) treatment fluid in the present invention can be purified by intensification filter progress, can recycle again, therefore Cost is greatly reduced, discharge of wastewater can also be reduced it is ensured that the feature of environmental protection of technique.
Brief description
Fig. 1 degumming process of the present invention flow chart;
Form after Boehmeria before processing in Fig. 2 embodiment 1:A is Boehmeria raw ramie before degumming process, and B is ramie after degumming process Flaxen fiber;Fig. 3 is form contrast before and after degumming process flow chart and fiber treatment.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content of present invention instruction, people in the art Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited Scope.
Embodiment 1
Sodium peroxide/carbamide/water is become treatment fluid with the proportions of mass ratio 10%/9%/81% and is cooled to -10 in advance DEG C, after net for the cleaning of Boehmeria raw ramie, it be laid on process on the net, and be immersed in 1min in precooling treatment liquid, apply mild mechanical simultaneously Pat, after process, fiber is cleaned with -10 DEG C for the treatment of fluids, treatment fluid reclaims.Fiber is washed to after neutrality in room temperature using 25 DEG C Lower natural drying.Boehmeria raw ramie before degumming process and the ramee after degumming process are as shown in Figure 2 A and 2B.Degumming 19.9 ± 5.9GPa of the relatively conventional technique of initial moduluss be reduced to 8.1 ± 3.2GP, degree of crystallinity obtains fiber by traditional handicraft 81.78% be reduced to 50.02%, regain brings up to 11.07% by 8.83%.Dyeability significance improves, and dyeing is deep Degree K/S value improves nearly 33.46%.
Embodiment 2
Lithium peroxide/thiourea/water quality is become degumming process liquid than the proportions for 10%/12%/78%, by Caulis et Folium Lini After raw ramie is cleaned, elaborate, spray process liquid online in processing, the raw ramie of liquid to be treated moistening is positioned over -5 DEG C of freezing processing 5min, fiber is subsequently cleaned by cooperative mechanical beating with -5 DEG C for the treatment of fluids simultaneously, and washing aftertreatment fluid reclaims, and fiber reuses 20 DEG C are washed to neutrality, then process in 50 DEG C of flash bakings.By the dyeability of fiber before and after contrast K cryogenic treatment, obtain The dye level K/S value of the flax fiber after process improves 101.4%.Flax fiber initial moduluss after process reduce 40.4%, illustrate that K cryogenic treatment can improve the pliability of flax fiber.
Embodiment 3
Potassium peroxide/carbamide/water quality is become degumming process liquid than the proportions for 9%/12%/79% and puts into leaching In groove, china-hemp fibers bundle applies treatment fluid by padding groove, and then fibre bundle is placed in -25 DEG C of freezing processing 30s, repeats to pad Refrigerating process 2 road, is padded rear cooperative mechanical and pats, process and using -5 DEG C for the treatment of fluids, fibre bundle is carried out, treatment fluid reclaims, Then fiber is washed to neutrality through 20 DEG C, and spontaneously dries at room temperature.Dyeing by fiber before and after contrast K cryogenic treatment Performance, the dye level K/S value of the china-hemp fibers after being processed improves 66.1%, the dyeing of china-hemp fibers after explanation process Performance gets a promotion.China-hemp fibers initial moduluss after process reduce 24.1%, illustrate that K cryogenic treatment can improve flax fiber Pliability.

Claims (9)

1. a kind of high-efficiency low-emission low temperature peroxidating retting method, including:
(1) by alkali-metal peroxide, amide substance and water mix, and obtain degumming process liquid;Wherein, alkali in degumming process liquid Metal peroxidess content is 0.5wt.%~20.0wt.%, and amide substance content is 0.5wt.%~20.0wt.%, remaining Measure as water;
(2) by treat degumming numb material adopt step (1) in degumming process liquid carry out degumming process;Wherein, the mode of process is Infiltrate, pad or spray, the condition of process is:1~10 road, per pass 10s~30min is processed under conditions of 5~-80 DEG C;
(3) material under 5~-20 DEG C of environment, degumming process in step (2) being obtained using the treatment fluid of preparation in step (1) Carry out just road cleaning, then clean to neutrality, be dried, obtain the numb material through high-efficiency low-emission low temperature peroxidating degumming.
2. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly in (1), alkali-metal peroxide is at least one in potassium peroxide, lithium peroxide and sodium peroxide.
3. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly in (1), amide substance is at least one in carbamide, thiourea, acetamide, caprolactam and tetraethylammonium chloride.
4. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly treat in (2) degumming numb material be Boehmeria, Fructus Cannabis, Caulis et Folium Lini, the raw ramie of Folium Agaves Sisalanae, Corchorus olitorius L. or Herba Apocyni veneti, flaxen fiber bundle or through just The flaxen fiber of step degumming process.
5. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly in (2), the processing mode of infiltration is:To treat that the immersion of degumming numb material reaches in the degumming process liquid for the treatment of temperature, coordinate simultaneously Mechanism is processed, and process sloughs treatment fluid through roll after terminating.
6. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly the processing mode padded in (2) is:To treat that degumming numb material, through degumming process liquid, is padded under processing conditions, leaching Roll rear cooperative mechanical effect to process.
7. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly in (2), the processing mode of spray is:Degumming process liquid is sprayed in treating, in degumming numb material, to be taken off under processing conditions Glue, cooperative mechanical effect in processing procedure is processed.
8. the method for the high-efficiency low-emission low temperature peroxidating retting according to any one in claim 5~7, its feature exists In described mechanism is beaten for machinery, mechanical oscillation or mechanical roll compacting.
9. a kind of method of high-efficiency low-emission low temperature peroxidating retting according to claim 1 is it is characterised in that described step Suddenly dry condition in (2) is:It is dried under 10~105 DEG C of normal pressures or vacuum environment.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106868607A (en) * 2017-03-23 2017-06-20 东华大学 A kind of high-efficiency low-emission low temperature peroxidating retting method
CN110409176A (en) * 2019-07-26 2019-11-05 青岛奥洛思新材料有限公司 A kind of production technology based on the modified Chinese fiber crops high grade cotton yarn fabric of biochemistry degumming

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1924120A (en) * 2006-09-11 2007-03-07 东华大学 Method of preparing fiber for weave by peroxide degumming method
WO2007037711A1 (en) * 2005-09-30 2007-04-05 Instytut Wlokien Naturalnych (Institute Of Natural Fibres) The method of fibrous plant degumming
CN102888726A (en) * 2012-10-17 2013-01-23 绍兴文理学院 Auxiliary-free refinement processing method of jute fiber
CN103993364A (en) * 2014-05-20 2014-08-20 东华大学 Method for enhancing property of ramie fiber through oxidative degumming
CN104562757A (en) * 2013-10-18 2015-04-29 天津天服三悦服装有限责任公司 Preparation method for silk cotton fabric

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007037711A1 (en) * 2005-09-30 2007-04-05 Instytut Wlokien Naturalnych (Institute Of Natural Fibres) The method of fibrous plant degumming
CN1924120A (en) * 2006-09-11 2007-03-07 东华大学 Method of preparing fiber for weave by peroxide degumming method
CN102888726A (en) * 2012-10-17 2013-01-23 绍兴文理学院 Auxiliary-free refinement processing method of jute fiber
CN104562757A (en) * 2013-10-18 2015-04-29 天津天服三悦服装有限责任公司 Preparation method for silk cotton fabric
CN103993364A (en) * 2014-05-20 2014-08-20 东华大学 Method for enhancing property of ramie fiber through oxidative degumming

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106868607A (en) * 2017-03-23 2017-06-20 东华大学 A kind of high-efficiency low-emission low temperature peroxidating retting method
CN110409176A (en) * 2019-07-26 2019-11-05 青岛奥洛思新材料有限公司 A kind of production technology based on the modified Chinese fiber crops high grade cotton yarn fabric of biochemistry degumming

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