CN110195263A - A kind of preparation method of solvent method production regenerated celulose fibre spinning glue - Google Patents

A kind of preparation method of solvent method production regenerated celulose fibre spinning glue Download PDF

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Publication number
CN110195263A
CN110195263A CN201910535997.3A CN201910535997A CN110195263A CN 110195263 A CN110195263 A CN 110195263A CN 201910535997 A CN201910535997 A CN 201910535997A CN 110195263 A CN110195263 A CN 110195263A
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dissolvers
solvent
layer
thick
preparation
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王维列
麦钮·瓦特·斯旦呢
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention discloses a kind of preparation methods of solvent method production regenerated fiber spinning glue, and by 2 or multiple vertical luwa evaporators and single horizontal tubular thick-layer evaporation dissolvers connection form.The aqueous mixture of cellulose and solvent and auxiliary agent is prepared into the cellulose spinning glue with spinnability, the mixtures of materials is first injected into 2 or multiple vertical luwa evaporators, be then injected into the horizontal tubular thick-layer dissolvers of coupled one and is evaporated and is mixed into regenerated celulose fibre spinning glue under vacuum.The present apparatus is suitable for carrying out the evaporation of large quantity of moisture in the case that first step medium viscosity is lower and the residence time is short using the good heat conductivity of luwa evaporator.Since viscosity is low, therefore the power consumption of motor is also accordingly greatly reduced.The present invention is able to achieve higher efficiency and guarantees the quality of uniform product, can also adjust production capacity according to the market demand.

Description

A kind of preparation method of solvent method production regenerated celulose fibre spinning glue
Technical field
The present invention relates to textile technology field, specifically a kind of solvent method produces regenerated celulose fibre spinning glue Preparation method.
Background technique
The regenerated celulose fibre glue of solvent method production at present mainly utilizes NMMO solvent to be mixed with cellulose to prepare. Now illustrated by taking the preparation process of lyocell (lyocell) fiber glue as an example.The preparation of Lyocell fibers glue is using nothing Malicious solvent NMMO(N- methyl morpholine-M- oxide) cellulose is directly carried out dissolution under physical change become it is highly viscous can The property spun glue.In order to realize this process, there are following three productions method, devices on Vehicles Collected from Market.
1. a kind of most widely used device is using luwa evaporator (also referred to as thin film evaporator) under vacuum conditions to containing There is the slurry congee of cellulose, water and NMMO and a small amount of auxiliary agent to carry out the evaporation of moisture, when the concentration of NMMO reaches 87% or so With regard to forming cellulose glue.Whole process is completed in luwa evaporator.A set of condenser system is separately configured in complete equipment, leads to The foundation for crossing measurement condensation water quantity to calculate the state of plastic and adjust as relevant temperature or rotor revolution number or vacuum degree.Then Glue carries out spinning to spinning machine by the subsequent processing such as pipeline and filtering.The advantages of luwa evaporator is that have well Heat transfer performance, but the disadvantage is that plant capacity is big, the time of material lagging is short, the bad control of glue uniformity.Due to equipment It is machined the limitation of aspect, large-sized processing equipment cannot infinitely amplify.In addition after amplifying to equipment, loading and larger, Requirement to workshop is also higher, causes cost of investment excessively high, and cost performance reduces.Maximum separate unit production capacity generally exists this equipment at present 15000 tons/year to 25000 tons/year.
2. another process units used on a small scale is that (also referred to as: kneading is anti-by horizontally disposed thick-layer dissolvers Answer device) under vacuum conditions to the evaporation containing cellulose, water and NMMO and the slurry congee progress moisture of a small amount of auxiliary agent, when NMMO's Cellulose glue is just formed when concentration reaches 87% or so.Whole process is completed in luwa evaporator and complete equipment A set of condenser system is separately configured.Then glue carries out spinning to spinning machine by the subsequent processing such as pipeline and filtering. The advantages of thick-layer dissolvers is that the material lagging time is longer, good mixing effect.The disadvantage is that high equipment cost, evaporation efficiency are low. Maximum separate unit production capacity is usually no more than 5000 tons/year to this equipment at present.The inadaptable needs being mass produced at present.
3. being to be combined use, such as patent application using the advantage of both the above device respectively there are also a kind of process units The patent of invention of the method for moulded parts " manufacture " entitled disclosed in publication No. CN104246029A, i.e. a luwa evaporator with One thick-layer dissolvers connection uses.Material as far as possible will be steamed in luwa evaporator using its good heat transfer performance more Shampoo divides and lower than at water evaporation quantity needed for glue, and then this slurry congee is evaporated to glue dissolution institute in thick-layer dissolvers on a small quantity The state of need simultaneously makes material be uniformly mixed into uniform glue using its excellent mixed performance.Although this device is than two kinds of front Equipment theoretically has certain advance, and the production capacity singly covered can also increase, but is still limited by luwa evaporator processing The limitation of size, therefore the requirement of more extensive production capacity cannot be reached.The limit production capacity of separate unit is no more than 30000 tons every year.It is a whole set of A set of condenser system is separately configured in equipment, does not determine the respective evaporation effect of each equipment and state by condensation water quantity, and It is the concentration of molding solution and/or diluent to be controlled by optical index (refraction index), and propose that ideally optical index is situated between Between 1.45-1.52, but this control method is only applicable in the single devices completion mentioned with above-mentioned 1 and 2 and entirely walks at glue Rapid situation, for 3 mention two kinds of equipment of combined use the case where cannot achieve.Belong to the significant deficiency in design, Cause a kind of situation for not having actual operation.The art does not have in production technology and equipment aspect since 2014 There is any technological improvement, can not enhance production capacities in the case where guaranteeing uniform glue.
Do not reach in view of the device list set ability of the above several types and produce 30000 tons of requirement per year, and mating more sets Prepare glue device also can inevitably be processed because of technology controlling and process and respectively same category of device itself processing present on difference and There is glue quality and difference occur, influences the homogeneity of end product quality.So needing to research and develop a kind of combination of bigger ability Device, so that the production capacity of every production line reaches the production capacity of 60000 tons annual (calculating for 330 days), it is even higher, it realizes higher Efficiency and the quality for guaranteeing uniform product, while there is operability.
Summary of the invention
It is an object of the invention to based in the understanding to above method advantage and disadvantage, proposing that a kind of production regeneration of solvent method is fine The preparation method of cellulose fiber spinning glue.It changes the configuration of operating procedure and equipment, to realize single line production capacity substantially It improves, while guaranteeing to obtain the spinning glue of preferably uniform solvent method preparation.Such as the production capacity of every production line is according to group Closing configuration can achieve 40000 tons of annual or 60000 tons annual (calculating for 330 days) production capacities.
To reach the purpose, list covering device needs to steam 2 or multiple (claiming below multiple) knifing according to production capacity Hair device and single thick film dissolvers are combined configuration.Instrument size is optimized according to production capacity.Each luwa evaporator And thick film dissolvers is required to individually be equipped with condenser system, is realized by measuring with actual evaporation water and calculated value Compare and to adjust the temperature of the collet heating agent of each single devices accordingly or adjust rotor revolution number or vacuum degree adjustment or knot It is adjusted altogether to control control of the evaporated water i.e. to glue dissolution degree.
Specific technical solution is as follows:
The preparation method of a kind of solvent method production regenerated celulose fibre spinning glue, by the aqueous of cellulose and solvent and auxiliary agent Mixture is prepared into the cellulose spinning glue with spinnability, it is characterised in that: by the mixtures of materials first inject 2 or Multiple vertical luwa evaporators are then injected into the horizontal tubular thick-layer dissolvers of coupled one and carry out under vacuum Evaporation and mixing.
Linkage section is using pump or spiral pusher or carries out material conveying by pipeline by gravity blanking mode or uses direct Mode
Each individually vertical luwa evaporator and tubular thick-layer dissolvers equipment monomer configure individual condenser system
Each individually vacuum system of vertical luwa evaporator and tubular thick-layer dissolvers can be separately configured or share or scrape Film evaporator shares a set of vacuum system
Each individually vertical luwa evaporator and tubular thick-layer dissolvers equipment monomer work under different vacuum pressures or It works on same vacuum pressure.
The solvent is other solvents of NMMO or dissolved cellulose.
Mixed material evaporation water and improves solvent strength in the vertical luwa evaporator, but molten lower than cellulose Concentration required for solving.
The solvent based on NMMO is such as used, NMMO is concentrated into the level higher than monohydrate.That is NMMO and water and NMMO Ratio be lower than 86.7%.
In the thick-layer evaporator, the material for being transported to the thick film dissolvers from luwa evaporator passes through evaporation Solvent concentration of ordinary dissolution is increased to by moisture can form spinnability glue with the level and homogenizing of cellulose dissolution.
The luwa evaporator jacket steam temperature is run between 100-180 degree, and preferably 100-150 degree is run, collet Hot water temperature runs between 80-105 degree.The thick film dissolvers collet heating agent is run between 90-120 degree, preferably 100- 110 degree.
The luwa evaporator and the thick film dissolvers are run under the vacuum of 40-100 absolute pressure vacuum degree, preferably 45- It is run under 55 absolute pressure vacuum degrees.
If luwa evaporator and the thick film dissolvers work under different vacuum degrees, the preferred vacuum of thick-layer dissolvers Pressure is less than the vacuum pressure of knifing dissolvers.
Evaporation process need to condense the vapor evaporated by condenser material under vacuum conditions.Utilize calculating Condensation water quantity and the comparison of practical condensation water quantity to adjust collet heat medium temperature or rotor speed or vacuum degree or in conjunction with controlling The degree that moisture is evaporated in spinning glue.Condensation number is needed as practical condensation number is less than to calculate, it can be by improving heat medium temperature Or increases rotor revolution number or reduce vacuum pressure or be used in combination to adjust.
By taking NMMO solvent as an example: the cellulose slurry congee containing NMMO being injected separately into multiple vertical luwa evaporators and is carried out Then prevapourising starches congee and is transported to evaporation in horizontal thick film dissolvers and mixes and be discharged after forming uniform glue.
Dissolution of the cellulose slurry congee in NMMO based on three kinds of known devices, from technology angle analysis containing NMMO Journey.
It was determined that course of dissolution can be basically divided into three steps.The first step is to evaporate water from cellulose-solvent slurry congee Point, until the dissolution starting point of cellulose.The starting point corresponds to and reaches dissolution window, corresponds to about 2.5 hydration NMMO.The step It needs a large amount of thermal energy to carry out evaporation water, but since cellulose was not yet dissolved without any additional residence time, and starches congee Viscosity it is lower.
After reaching dissolution window, the main dissolution that viscosity significantly increases is carried out in second step.The moisture phase of this step evaporation To less, it is evaporated to about 1.5 hydration NMMO always.
Third step then carries out less water evaporation by the homogenization degree of spinning glue and according to the concentration of cellulose It is determined to 0.8 to 1.0 hydrate.
The invention has the advantages that the present apparatus is lower suitable for first step medium viscosity using the good heat conductivity of luwa evaporator And the residence time it is short in the case where carry out large quantity of moisture evaporation.Since viscosity is low, thus the power consumption of motor also it is corresponding substantially It reduces.And thick-layer dissolvers then utilizes its excellent homogenize performance and longer residence time and suitable processing high viscosity object Characteristic and the moisture less situation of evaporation demand of material and be suitable for second step and third step, and be able to achieve higher efficiency and Guarantee the quality of uniform product, while there is operability.In addition, another outstanding advantages of this device are can basis User needs very big production capacity adjustment space, such as only opens a luwa evaporator, and others are not opened.Also it is conducive to tables of equipment simultaneously Solely is safeguarded and overhauled.This is extremely beneficial for control production scale.
Detailed description of the invention
Fig. 1 is device structure schematic diagram when 2 luwa evaporators correspond to a thick-layer dissolvers.
Device structure schematic diagram when Fig. 2 is 3 or multiple luwa evaporator one thick-layer dissolvers of correspondence.
1 is intake line I in figure, and 2. be intake line II, and 3 be luwa evaporator I, and 4 be luwa evaporator II, and 5 be condensation Device I, 6 be condenser II, and 7 be spiral pusher or direct-connected changeover portion, and 8 be pump or spiral pusher or direct-connected changeover portion, and 9 be thickness Film evaporator, 10 be condenser III.
Following embodiments by for the corresponding thick film dissolvers of two luwa evaporators to the features and advantages of the present invention into Row is illustrated;Attached drawing of the invention is not uniquely, it is one corresponding can to need to carry out multiple luwa evaporators according to client and production capacity Thick-layer dissolvers carries out different combination configurations.
Specific embodiment
Embodiment 1:
By intake line 1 and 2 wiped film vaporization quantitatively will be injected separately into NMMO and the auxiliary agent cellulose mixtures mixed in advance Device 3 and 4 can be separated also simultaneously and be carried out.
In luwa evaporator, the mixture material of injection occurs moisture and is concentrated by evaporation.The material of concentration is respectively from knifing Evaporator 3 and 4(can be carried out simultaneously, can also be separated and be carried out) it is transferred in the same corresponding thick-layer evaporator 9.
In luwa evaporator 3 and 4, collet heating in the case where, mixed material form a film from luwa evaporator and to Evaporation water under vacuum conditions during lower pusher, and cellulose does not reach dissolved state in the process.In thick-layer In dissolvers, in the case where collet heating, material is sufficiently mixed with solvent (NMMO) and evaporation section moisture reaches cellulose Dissolved state, to form highly viscous spinnability glue.Then the spinning glue is passed through by pipeline and pump by tapping equipment Body is transported to spinning machine and carries out spinning.
In order to further increase production capacity, cellulose concentration in glue can also slightly be improved, then be diluted again For the cellulose glue of suitable spinnability.It completes to dilute by input channel in tapping equipment.It can also be in tapping equipment Upstream disperses to carry out in the dilution of any position of thick film dissolvers or simultaneously in multiple positions.
Glue is transported to downstream processing and device for spinning by one or more pump in discharger downstream.
The secondary steam generated in luwa evaporator 3 and 4 and thick film dissolvers can by the condenser that accordingly connects into Row condensation.
Embodiment 2
By intake line 1 and 2 wiped film vaporization quantitatively will be injected separately into NMMO and the auxiliary agent cellulose mixtures mixed in advance Device 3 and 4 can be separated also simultaneously and be carried out.
Linkage section can be provided separately or first be focused on after one or more main pipelines to be connected with thick-layer dissolvers again.

Claims (15)

1. a kind of preparation method of solvent method production regenerated celulose fibre spinning glue, by containing for cellulose and solvent and auxiliary agent Aqueous mixtures are prepared into the cellulose spinning glue with spinnability, it is characterised in that: the mixtures of materials is first injected 2 Or multiple vertical luwa evaporators, be then injected into the horizontal tubular thick-layer dissolvers of coupled one and under vacuum into Row evaporates and is mixed into regenerated celulose fibre spinning glue.
2. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature exist In: the material conveying of vertical luwa evaporator and horizontal tubular thick-layer dissolvers uses pump or spiral pusher mode or falls by gravity Material mode carries out material conveying by pipeline or uses vertical luwa evaporator and the horizontal tubular thick-layer dissolvers side of being directly connected to Formula.
3. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature exist In: each individually vertical luwa evaporator and tubular thick-layer dissolvers equipment monomer configure individual condenser system.
4. according to the method described in claim 1, it is characterized by: each individually vertical luwa evaporator and tubular thick-layer are molten The vacuum system of solution device can be separately configured or share a set of vacuum system with luwa evaporator.
5. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature exist In: each individually vertical luwa evaporator and tubular thick-layer dissolvers equipment monomer work under different vacuum pressures or It works on same vacuum pressure.
6. the preparation method of the production of solvent method described in -5 regenerated celulose fibre spinning glue according to claim 1, feature Be: the solvent is other solvents of NMMO or dissolved cellulose.
7. method according to claim 1, it is characterised in that: mixed material evaporation water in the vertical luwa evaporator And solvent strength is improved, but lower than concentration required for cellulose dissolution.
8. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 7, it is characterised in that: The solvent based on NMMO is such as used, NMMO is concentrated into the level higher than monohydrate, i.e. NMMO is low with the ratio of water and NMMO In 86.7%.
9. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature exist In: in the thick-layer evaporator, the material for being transported to the thick film dissolvers from luwa evaporator passes through evaporation water Solvent concentration of ordinary dissolution, which is increased to, can form spinnability glue with the level and homogenizing of cellulose dissolution.
10. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature Be: the jacket steam temperature of the luwa evaporator is run between 100-180 degree, and preferably 100-150 degree is run, collet heat Coolant-temperature gage is run between 80-105 degree, and the thick film dissolvers collet heating agent is run between 90-120 degree, preferably 100-110 Degree.
11. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature exist In: the luwa evaporator and the thick film dissolvers are run under the vacuum of 40-100 absolute pressure vacuum degree, preferably 45-55 absolute pressure It is run under vacuum degree.
12. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 12, feature It is: if luwa evaporator and the thick film dissolvers work under different vacuum degrees, the preferred vacuum pressure of thick-layer dissolvers Power is less than the vacuum pressure of knifing dissolvers.
13. the preparation method of solvent method production regenerated celulose fibre spinning glue according to claim 1, feature exist In: evaporation process need to condense the vapor evaporated by condenser material under vacuum conditions, utilize the cold of calculating Condensate flow and the comparison of practical condensation water quantity are to adjust collet heat medium temperature or rotor speed or vacuum degree or in conjunction with controlling moisture In the degree of spinning glue evaporation, such as practical condensation number, which is less than to calculate, needs condensation number, can be by improving heat medium temperature or increasing Greater trochanter revolution reduces vacuum pressure or is used in combination to adjust.
14. the equipment in a kind of preparation method of solvent method production regenerated celulose fibre spinning glue as described in claim 1, Including vertical luwa evaporator and a horizontal tubular thick-layer dissolvers connected to it, it is characterised in that: 2 or multiple vertical Luwa evaporator is connect with a horizontal tubular thick-layer dissolvers.
15. the equipment in a kind of preparation method of solvent method production regenerated celulose fibre spinning glue as described in claim 1, It is characterized by: multiple vertical luwa evaporators are directly connected on horizontal tubular thick-layer dissolvers or first concentrate be connected to It is connected again with horizontal tubular thick-layer dissolvers after one main pipeline;Or vertical luwa evaporator is directly connected to horizontal tubular On thick-layer dissolvers, also have vertical luwa evaporator first concentrate be connected to a main pipeline after be connected to form again with thick-layer dissolvers Hybrid connections mode.
CN201910535997.3A 2019-06-20 2019-06-20 A kind of preparation method of solvent method production regenerated celulose fibre spinning glue Pending CN110195263A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112481708A (en) * 2019-09-11 2021-03-12 宁波国际材料基因工程研究院有限公司 High-flux polymer fiber preparation equipment and preparation method thereof

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DE102009061077A1 (en) * 2009-02-05 2011-06-22 List Holding Ag Separating material mixtures, particularly solutions, suspensions and emulsion, involves dividing main vaporization and degasification, where main vaporization and degasification are performed in separate mixing kneader
CN104246029A (en) * 2012-04-17 2014-12-24 利斯特股份公司 Method for producing moulded articles
KR20170085295A (en) * 2016-01-14 2017-07-24 에스케이이노베이션 주식회사 Purification Method by Decoloring and Crystallization of Anhydrous Sugar Alcohols
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Publication number Priority date Publication date Assignee Title
CH702321B1 (en) * 2006-05-12 2011-06-15 List Holding Ag Continuous direct evaporation and degassing of elastomer-containing polymer solution using heatable-mixing kneader, comprises concentrating elastomer-containing polymer solution, recovering and providing desired shape for further processing
DE102009061077A1 (en) * 2009-02-05 2011-06-22 List Holding Ag Separating material mixtures, particularly solutions, suspensions and emulsion, involves dividing main vaporization and degasification, where main vaporization and degasification are performed in separate mixing kneader
WO2011062600A1 (en) * 2009-11-19 2011-05-26 E. I. Du Pont De Nemours And Company Polycondensation with a kneader reactor
CN104246029A (en) * 2012-04-17 2014-12-24 利斯特股份公司 Method for producing moulded articles
KR20170085295A (en) * 2016-01-14 2017-07-24 에스케이이노베이션 주식회사 Purification Method by Decoloring and Crystallization of Anhydrous Sugar Alcohols
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112481708A (en) * 2019-09-11 2021-03-12 宁波国际材料基因工程研究院有限公司 High-flux polymer fiber preparation equipment and preparation method thereof
CN112481708B (en) * 2019-09-11 2022-08-12 宁波国际材料基因工程研究院有限公司 High-flux polymer fiber preparation equipment and preparation method thereof

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