CN116145449A - Lyocell fiber pulp fluffing liquid and preparation method thereof - Google Patents

Lyocell fiber pulp fluffing liquid and preparation method thereof Download PDF

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Publication number
CN116145449A
CN116145449A CN202211717313.XA CN202211717313A CN116145449A CN 116145449 A CN116145449 A CN 116145449A CN 202211717313 A CN202211717313 A CN 202211717313A CN 116145449 A CN116145449 A CN 116145449A
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China
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fluffing
solution
liquid
pulp
nmmo
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Inventor
郑柏山
刘勇
么志高
张东斌
周殿朋
杜占军
侯荣超
吴运生
韦吉伦
金杨
高云鹏
王海猛
殷权
王夏男
刘阳
王占山
陈欢
王晓磊
蔡泳进
张志军
卢方
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TANGSHAN SANYOU GROUP XINGDA CHEMICAL FIBER CO Ltd
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TANGSHAN SANYOU GROUP XINGDA CHEMICAL FIBER CO Ltd
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Priority to CN202211717313.XA priority Critical patent/CN116145449A/en
Publication of CN116145449A publication Critical patent/CN116145449A/en
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001Modification of pulp properties
    • D21C9/002Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives
    • D21C9/005Modification of pulp properties by chemical means; preparation of dewatered pulp, e.g. in sheet or bulk form, containing special additives organic compounds

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
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Abstract

The invention relates to a lyocell fiber pulp fluffing liquid and a preparation method thereof, belonging to the field of lyocell fiber production, and comprising the following steps: (1) Soaking pulp in NMMO solution with the temperature of 40-50 ℃ and the mass fraction of 70-76% and the conductivity of less than 100 mu s to obtain fluffing solution a; (2) Concentrating or squeezing the defibering liquid a to obtain defibering liquid b; (3) And mixing the fluffing solution b with an NMMO solution with the temperature of 76-85 ℃ and the mass fraction of 83-85% and fluffing uniformly to obtain cellulose fluffing solution c. According to the invention, NMMO solution is used for replacing water for impregnation, so that energy consumption is saved, unit productivity is improved, and the product quality of the produced lyocell fiber can be ensured.

Description

Lyocell fiber pulp fluffing liquid and preparation method thereof
Technical Field
The invention relates to a lyocell fiber pulp fluffing liquid and a preparation method thereof, belonging to the field of lyocell fiber production.
Background
The existing lyocell fiber dry process is required to crush dry pulp by adopting different methods according to different crushing size requirements, and as a great amount of dust is generated by crushing the dry pulp, potential safety hazards such as explosion exist, and mechanical damage is caused to cellulose molecules; the existing lyocell fiber wet process is characterized in that a large amount of water is required to be introduced to impregnate pulp to form pulp porridge containing 3-5% of cellulose, cellulose is further defibered, only 70% of water can be recycled, 30% of water is required to be discharged, 1 ton of pulp treatment water consumption is 18.8 tons according to 5% of concentration, 5.64 tons of discharged water is calculated according to 30%, 0.94 ton of fiber is taken away, 0.88 ton of the fiber comes from water supplementing, and the mass ratio of the fiber to the water is 50% through squeezing treatment: 50%, thus, NMMO solution with the mass fraction of 83% -85% which is 8-10 times of the mass of the relative fluffing solution is required to be mixed to form a proper mixture of fiber, NMMO and water. Thus, a large amount of water resources are consumed, the consumption of the NMMO solution with high concentration is large, and the production cost is high.
Disclosure of Invention
The invention aims to solve the technical problem of providing the lyocell fiber pulp fluffing liquid and the preparation method thereof, wherein NMMO solution is used for replacing water for impregnation, so that the energy consumption is saved, the unit productivity is improved, and the product quality of the produced lyocell fiber can be ensured.
The technical scheme for solving the technical problems is as follows: a preparation method of lyocell fiber pulp fluffing liquid comprises the following steps: (1) Soaking pulp in NMMO solution with the temperature of 40-50 ℃ and the mass fraction of 70-76% and the conductivity of less than 100 mu s to obtain fluffing solution a; (2) Concentrating or squeezing the defibering liquid a to obtain defibering liquid b; (3) And mixing the fluffing solution b with an NMMO solution with the temperature of 76-85 ℃ and the mass fraction of 83-85% and fluffing uniformly to obtain cellulose fluffing solution c.
On the basis of the technical scheme, the invention can be improved as follows.
Further, in the step (1), the bath ratio of the impregnation is 1:22-19.
Further, in the step (1), the soaking time is 20-50 minutes, so that pulp is fully soaked, and the fluffing solution a is obtained.
Further, in the step (2), the defibering liquid a is subjected to a press treatment using a belt press, a twin-roll press or a screw press.
Further, in the step (2), the mass ratio of cellulose, NMMO and water in the fluffing solution b is 15-25:52.5-59.5:22.5-25.5.
Further, in the step (3), the mass fraction of the NMMO solution with the mass fraction of 83-85% is 4-5 times of the mass of the fluffing solution b during mixing.
In the step (3), before the fluffing solution b is mixed with the NMMO solution with the mass fraction of 83% -85%, the fluffing solution b is hit and opened, and then is weighed, and the particles with the particle diameter smaller than 3cm are hit and opened.
Further, in the step (3), the mixing is carried out by stirring with a stirrer at a rotation speed of 120rpm for 10-15 minutes, and the reducing agent is further added during the mixing. The reducing agent is a mixture of propyl gallate and HA or hydroxylamine sulfate, the propyl gallate is usually added according to 0.5-1.5 kg/ton filament, the HA or hydroxylamine sulfate is usually added according to 0.2-0.6 kg/ton filament, and specific numerical values are judged and adjusted according to peak values of propyl gallate oxide, propyl gallate and formaldehyde reactant in the spinning solution.
Further, the mass fraction of cellulose of the untwining liquid a is 3-5%, the mass fraction of cellulose of the untwining liquid b is 15-25%, and the mass fraction of cellulose of the cellulose untwining liquid c is 10.5-12.5%.
The invention also provides a lyocell fiber pulp fluffing liquid, which is prepared by the preparation method of the lyocell fiber pulp fluffing liquid.
The beneficial effects of the invention are as follows:
(1) NMMO with the temperature of 40-50 ℃ and the mass fraction of 70-76% is directly mixed with pulp, and NMMO solution in the state has good permeability to fibers in the pulp, but has poor dissolving capacity, the NMMO at the moment has no capacity of enabling the fibers to rapidly break and swell, and the swelling process can uniformly occur in the whole fiber length direction, so that the NMMO solution has better uniformity and fewer large-particle-size fiber fragments; the NMMO solution for the subsequent mixing and fluffing is at a temperature of 76-85 ℃, which is prepared for the next step that the mixed solution enters a thin film evaporator to evaporate water and dissolve into glue. Therefore, the low-temperature NMMO impregnated fiber has more stable properties, and the high-temperature NMMO mixed fluffing is beneficial to subsequent further evaporation and densification.
(2) The conductivity of the NMMO solution for impregnation is less than 100 mu s, because too high conductivity accelerates NMMO decomposition, mainly radical reaction, polonowski reaction and N-O fracture, catalyzes Maillard reaction, the NMMO solution color deepens, catalyzes hydroxylamine decomposition under alkaline condition, and causes explosion; complexing with PG produces color, and the system safety is reduced, so the system conductivity is controlled.
(3) The NMMO solution is used for fluffing cellulose in pulp in a large bath ratio dipping mode to form fluffing solution a with the mass fraction of cellulose of 3-5%, so that the dust problem of a dry method is avoided, the site environment is good, the operation is safe, and the damage to cellulose molecules is small. The method adopts a large bath ratio impregnation mode, so that NMMO and cellulose are fully contacted, the impregnation effect of the cellulose is ensured, the viscosity of materials is low, the fiber defibering effect is good, and a temperature regulating system is not needed in equipment.
(4) The defibering solution a is subjected to concentration or squeezing treatment to form a defibering solution b, wherein the mass ratio of cellulose to NMMO to water is 15-25:52.5-59.5:22.5-25.5, because of containing more NMMO, NMMO solution with the temperature of 76-85 ℃ and the mass fraction of 83-85% can be directly mixed in the fluffing step, the fluffing effect is good, white cores are avoided, and the contact time of NMMO and cellulose is long, so that the cellulose swelling effect is guaranteed.
(5) The fluffing solution a with the mass fraction of 3-5% of cellulose is used for removing NMMO and water in a mechanical mode, a large amount of energy is saved in comparison with an evaporation mode, the mass fraction of cellulose is adjusted to 10.5-12.5% by using an NMMO solution with the mass fraction of 83-85% at the temperature of 76-85 ℃ while the fluffing solution b is formed, so that the load of solvent evaporation and glue preparation evaporation is prevented from being increased by introducing a large amount of water, and the parameters can be adjusted according to the evaporation capacity of the dissolution evaporation and glue preparation film, so that the dynamic matching of the whole line capacity is achieved, the equipment is easy to obtain, and the energy consumption is low.
Drawings
FIG. 1 is a schematic structural view of a device for producing a pulp fluffing liquid of a Seer fiber in the invention.
Detailed Description
The principles and features of the present invention are described below with examples given for the purpose of illustration only and are not intended to limit the scope of the invention.
As shown in fig. 1, the preparation method of the lyocell fiber pulp defibering solution is realized by a corresponding production device, firstly, NMMO solution with the mass fraction of 70-76% and the conductivity of less than 100 mu s is prepared in advance in a middle tank, raw materials can be prepared by adopting a spinning bath, commercially available concentrated NMMO solution and treated squeeze liquid, pulp (600 x 800-1000 x 750) is conveyed into an impregnation barrel by a pulp feeder or by using a pulp winding machine, the prepared NMMO solution with the mass fraction of 70-76% is conveyed into the impregnation barrel by a conveying pump and a heat exchanger (the temperature of the NMMO solution is controlled to be 40-50 ℃ by heat exchange of the heat exchanger) to be mixed, the impregnation is carried out according to the impregnation bath ratio of 1:22-19, then the mixture is conveyed into a pulp barrel to be continuously impregnated for 20-50 minutes, a good impregnation effect is achieved, and the defibering solution a with the mass fraction of cellulose of 3-5% is formed; the defibering liquid a is pumped to a squeezing device which can be a mesh belt type squeezer, a double-roller type squeezer or a screw extruder, the mass fraction of the pulp is squeezed to 15% -25% of cellulose to form the defibering liquid b, then the defibering liquid b is subjected to beating and opening treatment (the suspended opening drum of a cylindrical tooth comb opener can be used for beating and opening, the particle diameter of the solution is smaller than 3 cm), the solution is conveyed to a weighing device through a chute and a belt conveyor to be weighed, after accurate weighing, the solution is mixed with NMMO solution with the temperature of 76-85 ℃ and the mass fraction of 83% -85% at a pre-mixer, and is mixed and defibering again at the mixer, the mixer is provided with a stirrer with the rotating speed of 120rpm and the speed being relatively slow, the stirring and mixing time is 10-15 minutes, the fiber is mixed and defibering evenly, the reducing agent is added at the position, the cellulose defibering liquid c with the mass fraction of the pulp cellulose of 10.5-12.5% is finally pumped into a film evaporator of a dissolving unit through a single screw pump, and the glue is manufactured.
The reducing agent is a mixture of propyl gallate and HA or hydroxylamine sulfate, the propyl gallate is generally added according to 0.5-1.5 kg/ton silk, the HA or hydroxylamine sulfate is generally added according to 0.2-0.6 kg/ton silk, and specific numerical values are judged and adjusted according to peak values of propyl gallate oxide, propyl gallate and formaldehyde reactants in the spinning solution
The technical scheme of the invention is described below through each embodiment, wherein the percentages are mass fractions, and the corresponding proportions are mass ratios.
Example 1
Preparing 70% NMMO solution for standby before starting, preparing cosmo pulp, and feeding the cosmo pulp into a dipping barrel at a speed of 1.25 tons per hour, wherein the 70% NMMO solution is 21878.5 kg per hour, and the bath ratio is 19; during operation, 70% NMMO solution was consumed, 998 kg NMMO concentration 23% dope was used 21.7% and 3608 kg NMMO 83% concentrate The ratio of the solution is 78.3 percent, 9015.08 kg of NMMO solution with the concentration of 70 percent is prepared by mixing, the temperature is controlled at 40 ℃, and the conductivity is 80 mu s. Soaking pulp with 6% water (98% effective except water) and 70% NMMO solution for 20 min to form a fluffing solution a with cellulose mass fraction of 3-5%, squeezing to form fluffing solution b4606 kg, 25% of alpha-fibers (1151.5 kg), 52.5% of NMMO (2418.15 kg) and 22.5% of water (1036.35); adding 5407 kg of 76 ℃ and 83% NMMO solution (containing 4487.85 kg of NMMO), beating and opening, then mixing the mixture uniformly again in a pre-mixer (the rotation speed of the mixer is 120rpm, the mixing time is 10 minutes), adding a reducing agent, adjusting the mass fraction of cellulose in the pulp porridge to 11.5% (1151.5 kg), NMMO68.97% (6906.0 kg), and cellulose defibering liquid c10013.04 kg with water content of 19.53% (1955.5 kg), pumping the pulp porridge into a film evaporator to prepare glue through a single screw, heating and dehydrating 969 kg under negative pressure (namely, concentrating NMMO to 87.5% and water 969 kg, thereby forming 9044 kg of glue solution, 12.73% of methyl cellulose, MO76.36%, water content of 10.91%, and good glue forming effect and excellent spinnability.
Example 2
Compared with the example 1, the concentration of the NMMO solution is adjusted to 72 percent before starting, the equivalent squeezing degree is achieved, and the evaporation water of film evaporation is reduced by 79 kg
Preparing 72% NMMO solution for standby before starting, preparing cosmo pulp, and feeding the cosmo pulp into a dipping barrel at a speed of 1.25 tons per hour, wherein the 72% NMMO solution required for one hour is 21878.5 kg, and the bath ratio is 19; 72% NMMO solution was consumed during operation, 844.43 kg NMMO concentration 23% dope was used 18% by weight of the concentrate and 3761.57 kg of NMMO 83% strength concentrate The ratio is 82%, 9168.61 kg of NMMO solution with the concentration of 72% is prepared by mixing, the temperature is controlled at 50 ℃, and the conductivity is 90 mu s. Soaking pulp with 6% water (98% effective except water) and 70% NMMO solution for 30 min to form a fluffing solution a with cellulose mass fraction of 3-5%, squeezing to form fluffing solution b4606 kg, 25% of alpha-fibers (1151.5 kg), 54% of NMMO (2487.24 kg) and 21% of water (967.26 kg); adding 5407 kg of 80 ℃ and 83% NMMO solution (containing 4487.85 kg of NMMO), beating and opening, then mixing the mixture uniformly again in a pre-mixer (the rotation speed of the mixer is 120rpm, the mixing time is 15 minutes), adding a reducing agent, adjusting the mass fraction of cellulose in the pulp porridge to 11.5% (1151.5 kg), NMMO69.66% (6975.09 kg), cellulose defibering solution c10013.04 kg containing 18.84% (1886.46 kg) of water, pumping the pulp into a film evaporator to prepare the glue through a single screw, heating and dehydrating 890 kg of glue solution 9123.03 kg (namely, concentrating NMMO to 87.5% and needing 890 kg of distilled water) under negative pressure, wherein the content of methyl cellulose is 12.62%, NMMO76.46%, the content of water is 10.92%, the glue forming effect is good, and the spinnability is excellent.
Example 3
Compared with example 2, the squeezing degree is reduced by 5% by squeezing to 20%, and 145 kg of distilled water is needed in comparison with example 2.
Preparing 72% NMMO solution for standby before starting, preparing cosmo pulp, and feeding the cosmo pulp into a dipping barrel at a speed of 1.25 tons per hour, wherein the 72% NMMO solution required for one hour is 21878.5 kg, and the bath ratio is 19; 72% NMMO solution was consumed during operation, 1055.54 kg NMMO concentration 23% dope was used 18% by weight of the concentrate and 4701.96 kg of NMMO 83% strength concentrate The ratio is 82%, 8957.50 kg NMMO solution with concentration of 72% is prepared by mixing, the temperature is controlled at 45 ℃, and the conductivity is controlled85 mus. Soaking pulp with 6% water (98% effective except water) and 72% NMMO solution for 50 min to form a defibering solution a with cellulose mass fraction of 3-5%, squeezing to form a defibering solution b5757.50 kg, wherein 20% of alpha fibers (1151.5 kg), 57.6% NMMO (3316.32 kg) and 22.4% water (1289.68 kg) are formed; adding 4255.54 kg of 85 ℃ and 83% NMMO solution (containing 3532.10 kg of NMMO), beating and opening, mixing again in a pre-mixer uniformly (the rotation speed of the mixer is 120rpm, the mixing time is 15 minutes), adding a reducing agent, adjusting the mass fraction of cellulose in the pulp porridge to 11.5% (1151.5 kg), NMMO68.395% (6848.42 kg), and cellulose fluffing solution c10013.04 kg containing 20.105% (2013.12 kg) to prepare glue by pumping a single screw into a film evaporator, heating and dehydrating 1034.78 kg under negative pressure (namely, NMMO is concentrated to 87.5% and 1034.78 kg of distilled water), forming 8978.27 kg of glue solution containing 12.83% of alpha-fiber, NMMO76.28%, and water content of 10.90%, and having good glue forming effect and excellent spinnability.
According to the embodiments, the parameter adjustment has a large space, and the maximum glue making capability of the production line can be fully exerted.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.

Claims (10)

1. The preparation method of the lyocell fiber pulp fluffing liquid is characterized by comprising the following steps of: (1) Soaking pulp in NMMO solution with the temperature of 40-50 ℃ and the mass fraction of 70-76% and the conductivity of less than 100 mu s to obtain fluffing solution a; (2) Concentrating or squeezing the defibering liquid a to obtain defibering liquid b; (3) And mixing the fluffing solution b with an NMMO solution with the temperature of 76-85 ℃ and the mass fraction of 83-85% and fluffing uniformly to obtain cellulose fluffing solution c.
2. The method for preparing a lyocell fiber pulp fluffing liquid according to claim 1, wherein in the step (1), the bath ratio of impregnation is 1:22-19.
3. The method for preparing a fluffing liquid of lyocell fiber pulp according to claim 1, wherein in the step (1), the time of impregnation is 20 to 50 minutes, thereby obtaining fluffing liquid a.
4. The method for producing a lyocell fiber pulp defibering liquid according to claim 1, wherein in the step (2), the defibering liquid a is subjected to a press treatment using a belt press, a twin-roll press or a screw press.
5. The method for preparing a lyocell fiber pulp fluffing liquid according to claim 1, wherein in the step (2), the mass ratio of cellulose, NMMO and water in the fluffing liquid b is 15-25:52.5-59.5:22.5-25.5.
6. The method for preparing a lyocell fiber pulp fluffing liquid according to claim 1, wherein in the step (3), the mass fraction of the 83% -85% NMMO solution is 4-5 times the mass of fluffing liquid b during mixing.
7. The method for preparing a fluffing liquid of lyocell fiber pulp according to claim 6, wherein in the step (3), before the fluffing liquid b is mixed with the NMMO solution with the mass fraction of 83% -85%, the fluffing liquid b is hit and opened, and then is weighed, hit and opened until the particle diameter is less than 3cm.
8. The method for preparing a lyocell pulp fluffing solution according to claim 1, wherein in the step (3), the mixing is performed by using a stirrer, the rotation speed of the stirrer is 120rpm, the stirring and mixing time is 10-15 minutes, and a reducing agent is added during the mixing, wherein the reducing agent is a mixture of propyl gallate and HA or hydroxylamine sulfate, the propyl gallate is added at a rate of 0.5-1.5 kg/ton of silk, and the HA or hydroxylamine sulfate is added at a rate of 0.2-0.6 kg/ton of silk.
9. The method for preparing a lyocell fiber pulp fluffing liquid according to any one of claims 1 to 8, wherein the mass fraction of cellulose of fluffing liquid a is 3-5%, the mass fraction of cellulose of fluffing liquid b is 15-25%, and the mass fraction of cellulose fluffing liquid c is 10.5-12.5%.
10. A lyocell pulp fluffing solution, characterized in that the lyocell pulp fluffing solution is prepared by a preparation method of the lyocell pulp fluffing solution according to any one of claims 1-9.
CN202211717313.XA 2022-12-29 2022-12-29 Lyocell fiber pulp fluffing liquid and preparation method thereof Pending CN116145449A (en)

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