CN108004611A - A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice - Google Patents
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice Download PDFInfo
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- CN108004611A CN108004611A CN201711241914.7A CN201711241914A CN108004611A CN 108004611 A CN108004611 A CN 108004611A CN 201711241914 A CN201711241914 A CN 201711241914A CN 108004611 A CN108004611 A CN 108004611A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The present invention provides a kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, directly produces spinning solution using the NMMO solution comminuted cellulosics pulp of low concentration, swollen cellulose, dissolving cellulose.Using the technology can effective simplification of flowsheet, and then equipment investment is greatly lowered, production cost is reduced while energy-saving.Step is simple and convenient to operate, is highly practical.
Description
Technical field
The invention belongs to regenerated celulose fibre technical field, in particular to a kind of cellulose fiber by solvent method spinning
Stoste preparation method.
Background technology
Regenerated celulose fibre is the fiber produced with plant resources constantly regenerating in nature, is that one kind can be held
The regenerated resources of supervention exhibition.Increasingly deficient with petroleum resources, regenerated celulose fibre is due to excellent performance and can
Reproducibility, causes all the more the great attention of people.
The development of regenerated celulose fibre is generally divided into three phases, forms three generation products.The first generation was 20th century
The common viscose fiber just to emerge for solution shortage of cotton.The second generation is to start the 1950s to realize industrialized production
Koplon, product mainly include the toramomen (Polynosic) of Japan's research and development, the change type high humidity of American R ＆ D
Modulus fibre (HWM) and the Modal fibers of Lenzing companies of Austria production.Third generation product is with the 1990s
The short fibre Tencel (tencel) of release, the cellulose fiber by solvent method that long filament Newcell is representative.As developed country's environmental protection will
Ask it is increasingly stringent and fiber production cost sharply increase, the cellulose fibre of adhering process production the state such as American-European-Japanese just by
Gradually stop production, and be then generalized with short route, the cellulose fiber by solvent method of green processing characteristic；Recent year with
The raising of environmentally friendly cost, many viscose glue enterprises have aimed at the production of cellulose fiber by solvent method, and Some Enterprises have been realized in molten
The industrialized production of agent method cellulose fibre.
The preparation of cellulose fiber by solvent method spinning solution at present is all dense molten with NMMO after wet process using the paddle dregs of rice
Liquid mixes, and NMMO concentration is generally higher than 80%.Thus two problems can be produced, first, can be produced in paddle dregs of rice procedure for wet processing a large amount of
Waste water, causes production cost to improve；Second, in cellulose fiber by solvent method production process, solvent NMMO is that circulating repetition uses
, but the NMMO solution concentrations that collection is recycled from system are generally below 28%, and NMMO solution is concentrated by evaporation from low concentration
To high concentration, it is necessary to evaporate a large amount of water, big energy is consumed.Evaporation concentration equipment generally used now is all multi-effect evaporator,
Although with negative pressure, indirect steam make full use of, the technology such as UTILIZATION OF VESIDUAL HEAT IN, still need to consume a large amount of steam, while be concentrated by evaporation
During NMMO have a small amount of degraded, the color of solvent can deepen, so cause produce fibre whiteness reduce.
Yue Wentao on《Solvents N-methyl methylmorpholine-N-oxide (NMMO) recovery process and machine are used in Lyocell fiber production
The research of reason》It was found that in NMMO/ cellulose systems, acid condition and excessive temperature are unfavorable for the stabilization of NMMO, slurries
Keep the temperature standing time it is long, it will increase the degraded of NMMO, also can reinforcing fibre element degraded.Propylgallate is steady to system
Fixed optium concentration is 0.4wt%, itself and NaOH are used in combination as stabilizer, can improve system heat endurance and
Prevent the degraded of NMMO and cellulose.
The spinning solution preparation process of Chinese patent CN1336451 producing cellulose fibre through solvent.By pulp disintegrator
Comminuted fibres powder is in vacuum -9 × 104~-5 × 104Dry 6~12h, makes its moisture content under the conditions of Pa and 30~50 DEG C
Up to 2%~4%；By N-methyl morpholine oxide (NMMO) aqueous solution inspissation at reduced pressure conditions, make its water content equal to less than
15%；Above-mentioned powder and NMMO are stirred into 10~30min with certain proportion in a mixer under the conditions of 70~90 DEG C, formed light
Yellow paste, by the pastel feeding screw slenderness ratio be 1: 42~1: 52 double screw extruder in dissolving, deaeration 3~
The light brown clear solution generated after 15min is used for spinning.
But above-mentioned preparation method is complicated, production cost is high.
The content of the invention
In order to overcome above-mentioned deficiency, the present invention provides one kind and prepares cellulose fiber by solvent method spinning solution using the dry pulp dregs of rice
Method, spinning is directly produced using the NMMO solution comminuted cellulosics pulp of low concentration, swollen cellulose, dissolving cellulose
Stoste.Using the technology can effective simplification of flowsheet, and then equipment investment is greatly lowered, is reduced while energy-saving
Production cost.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, including：
(1) the NMMO solution containing NaOH is prepared；
(2) pulp is progressively put into the above-mentioned NMMO solution containing NaOH, is uniformly mixed, atherosclerotic mixture must be starched；
(3) it is swollen cellulose above-mentioned slurry atherosclerotic mixture dehydration by evaporation, then is mixed to the cellulose after swelling
Stabilizer and antioxidant are added in thing；It is uniformly mixed, obtains premix；
(4) premix be dehydrated, dissolved, deaeration, up to fiber spinning dope.
The application research is found：Compared with existing dissolution method indirectly, make cellulose that effectively swelling occur by pre-distillation
Afterwards, the dissolved efficiency and solubility of cellulose can be improved, while reduces gelular ion in produced spinning solution, extend spinning
Stoste filter screen usage time, reduce draping frequency, improves production efficiency and final cellulosic fibrous product quality.
Preferably, in step (1), the dry pulp dregs of rice refer to undressed pulp raw material, and pulp shape is piece fiber type element
Pulp or coiled material fiber type element pulp, pulp type source are the wooden oar dregs of rice, Cotton Pulp, bamboo pulp, straw pulp, hemp dissolving pulp, jade
The production cellulose fiber such as the rice core cellulose pulp Wesy paddle dregs of rice.
Preferably, the content (wt) of fiber pulp is 5%~12%, preferably 6%~8% in mixture.
Preferably, in step (1), NMMO solution concentrations (wt) are 40%~70%, preferably 45%~55%.
Different from prior art addition NaOH raisings NMMO stabilities of solution, the purpose that the present invention adds NaOH is that acceleration is molten
Wellabilities of the agent NMMO to cellulose.When the contents of NaOH in the solution are less than 0.01wt ‰, to solvent NMMO to cellulose
Wellability acceleration effect unobvious, when the contents of NaOH in the solution are more than 0.1wt ‰, continue increase NaOH dosage
It is little to liftings of the solvent NMMO to the wellability of cellulose, but cellulose is produced a small amount of degraded, while spinning can be caused
Stoste color burn influences fibre whiteness.Therefore, in step (1) of the present invention, contents of the preferable NaOH in NMMO solution
(wt) it is 0.01 ‰~0.1 ‰, more preferably 0.03 ‰~0.08 ‰.
Preferably, in step (3), vacuum is -90kpa~-99.9kpa, preferably -92kpa~-95kpa, dehydration by evaporation
Temperature be 50 DEG C~90 DEG C, preferable temperature be 65 DEG C~75 DEG C, the mixture after evaporation and concentration to reach static 30min top layers without
NMMO solution separates out, and into paste, micro- Microscopic observation occurs swollen fiber diameter and becomes larger mixture.
Preferably, in step (3), heat stabilizer be that propylgallate (PG) content is cellulose 0.05 ‰~
0.5 ‰, preferably 0.1 ‰~0.25 ‰；Antioxidant is that azanol (HA) content is 0.1 ‰~the 0.9 ‰ of cellulose, preferably
0.2 ‰~0.5 ‰；PG prepares mixed solution, PG contents (wt) 3 ‰~12 ‰, preferably 6 ‰ using the NMMO solution of step (1)
~8 ‰；HA uses the aqueous solution of 50% (wt), and PG and the HA continuous uniform all by the way of atomizing spray are added to cellulose
In mixture after swelling, premix is stirred to obtain by pre-mixing apparatus, premix temperature maintains 65 DEG C~85
DEG C, preferably 75 DEG C~80 DEG C.
The dissolver of the present invention use scraper film evaporator, be vertical equipment, material have at the top of into being dehydrated, be molten
Solution, deaeration integration, spinning solution are discharged from bottom.
Premix is continuously delivered in dissolver in step (4), vacuum ＞ -0.975MPa；Dissolving
The temperature zonal control of device, temperature subregion are more than 4th area, temperature of charge in accurate display device；One area's temperature of charge control exists
70 DEG C~90 DEG C, two areas temperature of charge controls are at 80 DEG C~95 DEG C, and the temperature of charge control of 3rd area is at 85 DEG C~100 DEG C, four area's things
Expect temperature control at 90 DEG C~105 DEG C；
Heat medium can select saturated vapor, high temperature heat conductive oil, biphenyl-biphenyl ether etc., preferably saturated vapor.
Present system research is found：For the premix that pre-distillation is dehydrated, temperature of charge is more than 110 DEG C
When, degradation rate is fast, and the degree of polymerization is relatively low, and steam utilization is low.Therefore, the premix that the present invention is dehydrated based on pre-distillation
Specific moisture content and degradation rate, find by large scale experiment：Set that (area's temperature of charge control is at 70 DEG C using four-temperature region
~90 DEG C, two areas temperature of charge controls are at 80 DEG C~95 DEG C, and the temperature of charge control of 3rd area is at 85 DEG C~100 DEG C, four area's material temperature
Degree control is at 90 DEG C~105 DEG C), to ensure that premix lower part 1/5 is being degraded, but no more than 1/4 (otherwise there is danger)；
Realize at a lower temperature, the high quality of spinning solution, quick preparation.
Present invention also offers cellulose fibre spinning solution prepared by any above-mentioned method.
Present invention also offers any cellulose fibre spinning solution answering in regenerated celulose fibre is prepared
With.
Beneficial effects of the present invention
(1) present invention need not crush the dry pulp dregs of rice, effectively prevent generation dust band in dry pulp dregs of rice crushing process
The problem of carrying out security risk.The NMMO solution concentrations that the present invention uses are relatively low, reduce solvent concentration equipment investment, simultaneously because
NMMO solution thickening temperatures effectively reduce, and avoid the phenomenon that NMMO decomposes in evaporating concentration process.The present invention is not required to
Wet-treating is carried out to pulp, reduces wastewater discharge.
(2) preparation method of the present invention is simple, production efficiency is high, highly practical, easy to spread.
Embodiment
It is noted that described further below is all illustrative, it is intended to provides further instruction to the application.It is unless another
Indicate, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, step are as follows：
(1) will the dry pulp dregs of rice put into NMMO solution in, under the action of mechanical external force crush be made homogeneous cellulose/
NMMO/H2O mixtures；
(2) by said mixture, heating evaporation removes partial moisture under vacuum, makes cellulose that Swelling occur；
(3) heat stabilizer and antioxidant are added into the cellulose mixing being swollen, be thoroughly mixed to form homogeneous steady
Fixed premix；
(4) premix is dehydrated, deaeration, cellulose dissolution forms the transparent spinning solution of stable homogeneous.
In the present invention, the dry pulp dregs of rice refer to undressed pulp raw material in step (1), and pulp shape can be piece type fibre
The plain pulp of dimension or coiled material fiber type element pulp, pulp type source can be the wooden oar dregs of rice, Cotton Pulp, bamboo pulp, straw pulp, fiber crops
The production cellulose fiber such as pulp, the corn cob fiber element pulp Wesy paddle dregs of rice.The content (wt) for mixing fiber pulp in story is 5%
~12%, preferably 6%~8%.
In the present invention, NMMO solution concentrations (wt) are 40%~70%, preferably 45%~55% in step (1), in solution
Suitable NaOH is added to improve the stability of NMMO, the contents (wt) of NaOH in the solution are 0.01 ‰~0.1 ‰, preferably
0.03 ‰~0.08 ‰.
In the present invention, mechanical force is the mechanical external force that hydrabrusher provides in step (1), uses the excellent of hydrabrusher
Point is that the dry pulp dregs of rice are not required mechanical lapping to crush, and is not in capillary fiber dust, prevents the security risk in production；Waterpower is broken
Temperature control during pulp grinder crushing pulp is at 45 DEG C~70 DEG C, preferably 50 DEG C~60 DEG C.
In the present invention, vacuum is -90kpa~-99.9kpa, preferably -92kpa~-95kpa in step (2), and evaporation is de-
Coolant-temperature gage is 50 DEG C~90 DEG C, and preferable temperature is 65 DEG C~75 DEG C, can meet production requirement within this range, and can be reduced pair
The requirement of equipment, while be conducive to the maintaining of equipment；Mixture after evaporation and concentration to reach static 30min top layers without
NMMO solution separates out, and into paste, micro- Microscopic observation occurs swollen fiber diameter and becomes larger mixture.
In the present invention, heat stabilizer is that propylgallate (PG) content is the 0.05 ‰ of cellulose in step (3)
~0.5 ‰, preferably 0.1 ‰~0.25 ‰；Antioxidant is that azanol (HA) content is 0.1 ‰~the 0.9 ‰ of cellulose, excellent
Select 0.2 ‰~0.5 ‰；PG using step (1) NMMO solution prepare mixed solution, PG contents (wt) 3 ‰~12 ‰, preferably
6 ‰~8 ‰；HA uses the aqueous solution of 50% (wt), and PG and the HA continuous uniform all by the way of atomizing spray are added to fibre
In mixture after dimension element swelling, premix is stirred to obtain by pre-mixing apparatus, premix temperature maintains 65 DEG C
~85 DEG C, preferably 75 DEG C~80 DEG C.
In the present invention, premix is continuously delivered in dissolver in step (4), vacuum want ＞-
0.975MPa；The temperature of dissolver wants zonal control, and temperature subregion is greater than 4th area, material temperature in accurate display device
Degree；At 70 DEG C~90 DEG C, preferably 80 DEG C~85 DEG C, two area's temperature of charge are controlled at 80 DEG C~95 DEG C the temperature of charge control of one area,
It is preferred that 85 DEG C~90 DEG C, at 85 DEG C~100 DEG C, preferably 90 DEG C~95 DEG C, four areas' temperature of charge control the temperature of charge control of 3rd area
At 90 DEG C~105 DEG C, preferably 95 DEG C~100 DEG C；Heat medium can select saturated vapor, high temperature heat conductive oil, biphenyl-biphenyl ether
Deng preferred saturated vapor.
Embodiment 1
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, step are as follows：
The NMMO solution of 45% (wt) is added in the broken oarage of waterpower first, heating-up temperature is 50 DEG C；To NMMO solution
The NaOH solution of 32% (wt) of middle addition, final NaOH contents in mixed liquor are 0.03 ‰；Then it is 653 the degree of polymerization, contains
The pulp of water rate 6.21% (wt) is progressively put into NMMO solution, cellulose oven-dry weight and the mass ratio of NMMO in solution in pulp
1:7.8 preparating mixtures, are mixed 30min, and material forms homogeneous slurry atherosclerotic mixture, wherein content of cellulose
5.43%.By blending transportation into vacuum evaporator, vacuum is -95KPa, temperature is 75 DEG C, and being evaporated dehydration makes fibre
Dimension element is swollen, at this time content of cellulose 9.4% in mixture.Mixed by way of atomizing spray to the cellulose after swelling
50% (wt) HA aqueous solutions and 6 ‰ (wt) PG mixed liquors are added in compound, HA and PG additions are respectively cellulose
0.2 ‰ and 0.1 ‰, premix is obtained after being thoroughly mixed.Premix is delivered to dissolver by starching congee delivery pump,
Dissolver is heated using saturated vapor, and vacuum is -0.98MPa, one to four area's temperature of charge is respectively 81 DEG C, 85.5 DEG C,
92 DEG C and 96 DEG C, it is dehydrated, dissolves, spinning solution is made in deaeration, content of cellulose 9.9% in spinning solution, viscosity 3894Pa.s.
Embodiment 2
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, step are as follows：
The NMMO solution of 50% (wt) is added in the broken oarage of waterpower first, heating-up temperature is 55 DEG C；To NMMO solution
The NaOH solution of 32% (wt) of middle addition, final NaOH contents in mixed liquor are 0.04 ‰；Then it is 749 the degree of polymerization, contains
The pulp of water rate 6.15% (wt) is progressively put into NMMO solution, cellulose oven-dry weight and the mass ratio of NMMO in solution in pulp
1:7.0 preparating mixtures, are mixed 35min, and material forms homogeneous slurry atherosclerotic mixture, wherein content of cellulose
6.63%.By blending transportation into vacuum evaporator, vacuum is -93KPa, temperature is 72 DEG C, and being evaporated dehydration makes fibre
Dimension element is swollen, at this time content of cellulose 10.36% in mixture.To the cellulose after swelling by way of atomizing spray
50% (wt) HA aqueous solutions and 7 ‰ (wt) PG mixed liquors are added in mixture, HA and PG additions are respectively cellulose
0.25 ‰ and 0.15 ‰, premix is obtained after being thoroughly mixed.Premix is delivered to dissolving dress by starching congee delivery pump
Put, dissolver is heated using saturated vapor, and vacuum is -0.98MPa, and one to four area's temperature of charge is respectively 81.5 DEG C, 87
DEG C, 93 DEG C and 96 DEG C, dehydration, dissolving, deaeration are made spinning solution, content of cellulose 10.95% in spinning solution, viscosity
11560Pa.s。
Embodiment 3
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, step are as follows：
The NMMO solution of 55% (wt) is added in the broken oarage of waterpower first, heating-up temperature is 60 DEG C；To NMMO solution
The NaOH solution of 32% (wt) of middle addition, final NaOH contents in mixed liquor are 0.04 ‰；Then it is 653 the degree of polymerization, contains
The pulp of water rate 6.21% (wt) is progressively put into NMMO solution, cellulose oven-dry weight and the mass ratio of NMMO in solution in pulp
1:6.4 preparating mixtures, are mixed 40min, and material forms homogeneous slurry atherosclerotic mixture, wherein content of cellulose
7.92%.By blending transportation into vacuum evaporator, vacuum is -95KPa, temperature is 80 DEG C, and being evaporated dehydration makes fibre
Dimension element is swollen, at this time content of cellulose 11.30% in mixture.To the cellulose after swelling by way of atomizing spray
50% (wt) HA aqueous solutions and 8 ‰ (wt) PG mixed liquors are added in mixture, HA and PG additions are respectively cellulose
0.3 ‰ and 0.2.5 ‰, obtains premix after being thoroughly mixed.Premix is delivered to dissolving dress by starching congee delivery pump
Put, dissolver is heated using saturated vapor, and vacuum is -0.98MPa, and one to four area's temperature of charge is respectively 82.5 DEG C, 87
DEG C, 94 DEG C and 99 DEG C, dehydration, dissolving, deaeration are made spinning solution, content of cellulose 12.1% in spinning solution, viscosity
14830Pa.s。
Embodiment 4
A kind of method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, step are as follows：
The NMMO solution of 60% (wt) is added in the broken oarage of waterpower first, heating-up temperature is 50 DEG C；To NMMO solution
The NaOH solution of 32% (wt) of middle addition, final NaOH contents in mixed liquor are 0.02 ‰；Then it is 548 the degree of polymerization, contains
The pulp of water rate 6.08% (wt) is progressively put into NMMO solution, cellulose oven-dry weight and the mass ratio of NMMO in solution in pulp
1:5.8 preparating mixtures, are mixed 45min, and material forms homogeneous slurry atherosclerotic mixture, wherein content of cellulose
9.32%.By blending transportation into vacuum evaporator, vacuum is -95KPa, temperature is 80 DEG C, and being evaporated dehydration makes fibre
Dimension element is swollen, at this time content of cellulose 12.2% in mixture.To the cellulose after swelling by way of atomizing spray
50% (wt) HA aqueous solutions and 6.5 ‰ (wt) PG mixed liquors are added in mixture, HA and PG additions are respectively cellulose
0.15 ‰ and 0.1 ‰, after being thoroughly mixed premix.Premix is delivered to dissolving dress by starching congee delivery pump
To put, dissolver is heated using saturated vapor, and vacuum is -0.98MPa, one to four area's temperature of charge is respectively 82.5 DEG C,
87.5 DEG C, 92.5 DEG C and 96.5 DEG C, dehydration, dissolving, deaeration are made spinning solution, content of cellulose 12.9% in spinning solution,
Viscosity 16020Pa.s.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, this hair is not limited to
Bright, although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it is still
It can modify to the technical solution described in previous embodiment, or equivalent substitution is carried out to which part.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on, should be included in protection scope of the present invention
Within.Although the above-mentioned embodiment to the present invention is described, not limiting the scope of the invention, institute
Belong to field technology personnel and should be understood that on the basis of technical scheme those skilled in the art need not pay wound
The various modifications or deform still within protection scope of the present invention that the property made work can be made.
Claims (10)
- A kind of 1. method that cellulose fiber by solvent method spinning solution is prepared using the dry pulp dregs of rice, it is characterised in that including：(1) NMMO solution is prepared；(2) pulp is progressively put into the above-mentioned NMMO solution containing NaOH, is uniformly mixed, atherosclerotic mixture must be starched；(3) it is swollen cellulose above-mentioned slurry atherosclerotic mixture dehydration by evaporation, then into the cellulose mixtures after swelling Add stabilizer and antioxidant；It is uniformly mixed, obtains premix；(4) premix be dehydrated, dissolved, deaeration, up to fiber spinning dope.
- 2. the method as described in claim 1, it is characterised in that in step (2), the dry pulp dregs of rice refer to undressed pulp former material Material, pulp shape are piece fiber type element pulp or coiled material fiber type element pulp, pulp type source be the wooden oar dregs of rice, Cotton Pulp, The production cellulose fiber such as bamboo pulp, straw pulp, hemp dissolving pulp, the corn cob fiber element pulp Wesy paddle dregs of rice.
- 3. the method as described in claim 1, it is characterised in that slurry atherosclerotic mixture in fiber pulp content for 5wt%~ 12wt%, preferably 6wt%~8wt%.
- 4. the method as described in claim 1, it is characterised in that in step (1), NMMO solution concentrations (wt) for 40wt%~ 70wt%, preferably 45wt%~55wt%.
- 5. the method as described in claim 1, it is characterised in that in step (1), the content of NaOH in the NMMO solution containing NaOH For ‰~0.1wt of 0.01wt ‰, preferably ‰~0.08wt of 0.03wt ‰.
- 6. the method as described in claim 1, it is characterised in that in step (3), the condition of dehydration by evaporation is：Vacuum for- 90kpa~-99.9kpa, preferably -92kpa~-95kpa, dehydration by evaporation temperature be 50 DEG C~90 DEG C, preferable temperature for 65 DEG C~ 75 DEG C, the mixture after evaporation and concentration will reach static 30min top layers and be separated out without NMMO solution, and mixture is into paste, microscope Lower observation occurs swollen fiber diameter and becomes larger.
- 7. the method as described in claim 1, it is characterised in that in step (3), heat stabilizer contains for propylgallate (PG) Measure 0.05 ‰ for cellulose~0.5 ‰, preferably 0.1 ‰~0.25 ‰；Antioxidant is that azanol (HA) content is fiber The 0.1 ‰ of plain weight~0.9 ‰, preferably 0.2 ‰~0.5 ‰；PG prepares mixed solution, PG using the NMMO solution of step (1) Content (wt) 3 ‰~12 ‰, preferably 6 ‰~8 ‰；HA uses the aqueous solution of 50% (wt), and PG and HA are using atomizing spray Being added in the mixture after cellulose is swollen for mode continuous uniform, premix is stirred to obtain by pre-mixing apparatus, Premix temperature maintains 65 DEG C~85 DEG C, preferably 75 DEG C~80 DEG C.
- 8. the method as described in claim 1, it is characterised in that in step (4), the dissolver of premix is thin for scraper-type Film evaporator, temperature zonal control, temperature subregion are more than 4th area, temperature of charge in accurate display device；The temperature of charge control of one area System is at 70 DEG C~90 DEG C, and the temperature of charge control of 2nd area is at 80 DEG C~95 DEG C, and three area's temperature of charge controls are at 85 DEG C~100 DEG C, four Area's temperature of charge control is at 90 DEG C~105 DEG C；Heat medium can select saturated vapor, high temperature heat conductive oil, biphenyl-biphenyl ether etc., preferably saturated vapor.
- 9. cellulose fibre spinning solution prepared by claim 1-8 any one of them method.
- 10. application of the cellulose fibre spinning solution described in claim 9 in regenerated celulose fibre is prepared.
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| CN110205691A (en) * | 2019-06-28 | 2019-09-06 | 上海建沪鸿达科技有限公司 | A kind of dissolvant type nanofiber spinning solution |
| CN110396222A (en) * | 2018-04-24 | 2019-11-01 | 恒天纤维集团有限公司 | A kind of preparation method of cellulose mixing slurry |
| CN110699769A (en) * | 2019-11-18 | 2020-01-17 | 武汉纺织大学 | Method for preparing lyocell fibers by using ramie fibers as raw materials |
| CN112981642A (en) * | 2021-02-06 | 2021-06-18 | 福建宏远集团有限公司 | Preparation method of bamboo/cotton blended fiber yarn |
| CN114016141A (en) * | 2021-12-09 | 2022-02-08 | 赛得利(常州)纤维有限公司 | Method for preparing fiber spinning solution by direct dissolution method |
| CN114214784A (en) * | 2021-12-10 | 2022-03-22 | 湖南俏妃卫生用品有限公司 | Preparation method of bamboo fiber and corn fiber bi-component non-woven fabric |
| CN116120597A (en) * | 2019-10-17 | 2023-05-16 | 武汉纺织大学 | Method for rapidly dissolving cellulose by NMMO alcohol solution |
| CN116254619A (en) * | 2022-12-19 | 2023-06-13 | 山东金英利新材料科技股份有限公司 | Wool protein/cellulose composite Lyocell fiber and preparation method thereof |
| CN116356441A (en) * | 2023-03-02 | 2023-06-30 | 东华大学 | Preparation method of regenerated cellulose fiber based on corncob |
| CN116854996A (en) * | 2023-09-01 | 2023-10-10 | 保定天鹅新型纤维制造有限公司 | Cellulose mixed pulp and preparation method thereof |
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| CN110396222A (en) * | 2018-04-24 | 2019-11-01 | 恒天纤维集团有限公司 | A kind of preparation method of cellulose mixing slurry |
| CN108893796A (en) * | 2018-06-29 | 2018-11-27 | 百事基材料（青岛）股份有限公司 | A kind of plant source modified cellulose fibre |
| CN110205691A (en) * | 2019-06-28 | 2019-09-06 | 上海建沪鸿达科技有限公司 | A kind of dissolvant type nanofiber spinning solution |
| CN116120597A (en) * | 2019-10-17 | 2023-05-16 | 武汉纺织大学 | Method for rapidly dissolving cellulose by NMMO alcohol solution |
| CN110699769A (en) * | 2019-11-18 | 2020-01-17 | 武汉纺织大学 | Method for preparing lyocell fibers by using ramie fibers as raw materials |
| CN110699769B (en) * | 2019-11-18 | 2022-05-20 | 保定澳森制衣股份有限公司 | Method for preparing lyocell fibers by using ramie fibers as raw materials |
| CN112981642A (en) * | 2021-02-06 | 2021-06-18 | 福建宏远集团有限公司 | Preparation method of bamboo/cotton blended fiber yarn |
| CN114016141A (en) * | 2021-12-09 | 2022-02-08 | 赛得利(常州)纤维有限公司 | Method for preparing fiber spinning solution by direct dissolution method |
| CN114214784A (en) * | 2021-12-10 | 2022-03-22 | 湖南俏妃卫生用品有限公司 | Preparation method of bamboo fiber and corn fiber bi-component non-woven fabric |
| CN116254619A (en) * | 2022-12-19 | 2023-06-13 | 山东金英利新材料科技股份有限公司 | Wool protein/cellulose composite Lyocell fiber and preparation method thereof |
| CN116356441A (en) * | 2023-03-02 | 2023-06-30 | 东华大学 | Preparation method of regenerated cellulose fiber based on corncob |
| CN116854996A (en) * | 2023-09-01 | 2023-10-10 | 保定天鹅新型纤维制造有限公司 | Cellulose mixed pulp and preparation method thereof |
| CN116854996B (en) * | 2023-09-01 | 2023-11-03 | 保定天鹅新型纤维制造有限公司 | Cellulose mixed pulp and preparation method thereof |
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