CN101240461A - Method for preparing cellulose spinning fluid - Google Patents
Method for preparing cellulose spinning fluid Download PDFInfo
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- CN101240461A CN101240461A CNA2007100637448A CN200710063744A CN101240461A CN 101240461 A CN101240461 A CN 101240461A CN A2007100637448 A CNA2007100637448 A CN A2007100637448A CN 200710063744 A CN200710063744 A CN 200710063744A CN 101240461 A CN101240461 A CN 101240461A
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Abstract
The invention relates to a preparation method of cellulose spinning solution, including a mixed solvent with low boiling point, volatile, polar organic solvent as a promoter and the N-methylmorpholine-N oxides (NMMO) of 8-18% moisture content; the cellulose pulp is mixed with the mixed solvent forming a uniform mixed materials; the low boiling point volatile organic solvent is removed from the mixed materials and the low content is lower than 5%, the cellulose of mixed materials is dissolved in the NMMO forming the cellulose spinning solution under heating. The invention is used the promoter delaying swelling and preventing premature dissolution of cellulose to reduce the solvent viscosity, the cellulose is dissolved uniformly, completely, the advantage which the pulp is impregnated directly in the high concentration solvent, and overcomes the abuse of uneven mixed, the used promoter is easy to extract and to recycle.
Description
Technical field
The present invention relates to a kind of preparation method of cellulose spinning fluid, particularly cellulose pulp is dissolved in the method that forms spinning solution in N-methylmorpholine-N oxide (NMMO), belong to textile technology field.
Background technology
Carry out nontoxic spinning produce cellulose fibers as solvent, delivered up to a hundred patents with N-methylmorpholine-N oxide (NMMO).But from dissolution process, nothing more than following two kinds of methods.
A kind of method be with in concentration NMMO (moisture content is 20-60%) mix with cellulose pulp and make slurry congee earlier, by the dissolution kettle of thin film evaporator formula, under vacuum and heating, remove unnecessary moisture content then, make system enter dissolved state.As patent US 509469, CN 1181788, and CN 1072284, WO 94/653 etc., and this method is used on industrial production.The patent that yet has is not used the dissolution kettle of thin film evaporator formula, and uses the dissolution kettle of similar kneader formula to carry out the vacuum dehydration dissolving, and as US 4246221, US 4416698, and CN 1501990, CN 111161C, and CN 1435529, CN 1449460 etc.This method is used on the device of some pilot-scales, but large-scale production yet there are no the report of use.
Another kind method is directly to mix with cellulose pulp with high concentration NMMO (moisture content is 8-15%), because system does not have unnecessary moisture content, need not therefore can directly add the hot extrusion dissolving with screw extruder through the process of dehydration.Earlier cellulose pulp is ground into Powderedly as CN 1336451, mixes less than 15% NMMO with moisture content again, directly dissolve then with the twin (double) screw extruder extruding.CN 1468889 similarly, earlier cellulose pulp is pulverized powder into about the 1mm size, be 12% NMMO again with moisture content, two charging apertures from twin (double) screw extruder quantitatively add in proportion respectively, mix in twin (double) screw extruder, heating and extruding dissolving.CN 1435529 then elder generation is 13.3% NMMO heating and melting with moisture content, and quenching to 50 ℃ is made over-cooled solution, mixes with cellulose pulp in twin shaft swollen mixt maker, enters a single screw extrusion machine then and extrudes dissolving.The advantage of this method is to have saved dehydration, can shorten dissolution time, helps reducing the decomposition of solvent.But shortcoming is solvent and cellulose pulp to be difficult to mix, and it is more difficult particularly to prepare the higher spinning solution of cellulose concentration.
KR20010093598 discloses a kind of preparation method of cellulose spinning fluid, it adopts and contains the NMMO ORGANIC SOLVENT MIXTURES swollen cellulose that is at least 25% methyl alcohol, ethanol or acetone, reduction vaporization organic solvent to the content of organic solvent is 5-20%, dissolving cellulos simultaneously fully is in bathing with dissolved cellulose solution deaeration, filtration, with spinning solution direct fabrics to organic solvent.This invention adopts methyl alcohol, ethanol or acetone place of water to combine with NMMO, because the strong absorptive of NMMO, realize that anhydrous NMMO is difficult with the mixing ratio of appeal organic solvent, and adopt organic solution will use a large amount of appeal volatile organic solvents as coagulating bath, increase to some extent on the cost, also brought new difficulty in the operation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of cellulose spinning fluid, this method can guarantee that solvent mixes with the even of cellulose pulp, need not dehydration again, the cellulose spinning fluid that obtains mixing need not to change existing spinning technique and directly carries out spinning.
In order to realize the object of the invention, the invention provides a kind of preparation method of cellulose spinning fluid, may further comprise the steps:
(1) be that N-methylmorpholine-N oxide (NMMO) of 8-18% mixes and forms a mixed solvent with low boiling, volatility, polar organic solvent as auxiliary agent and moisture content;
(2) cellulose pulp is mixed formation one even mixed materials with mixed solvent;
(3) the low boiling volatile organic solvent is removed from mixed material, be lower than 5% to the content of low boiling volatile organic solvent.
(4) mixed material is sent in the dissolution equipment processing and be dissolved in NMMO fully, obtain cellulose spinning fluid until cellulose.
Among the above-mentioned preparation method of the present invention, with cellulose pulp mix with mixed solvent form a mixed material after, also can comprise the mixed material device that mixed material is placed controllable temperature, and stir even until mixing of materials.This mixed material device can be the vertical or horizontal mixing kettle of the band stirring of being furnished with chuck and temperature control.
Among the present invention, the addition of cellulose pulp can be the 10-20% of the NMMO consumption of moisture content 8-18%, and the consumption of polar organic solvent can be 0.2-2.0 times of cellulose.
Among the present invention, is that N-methylmorpholine-N oxide (NMMO) of 8-18% mixes and forms a mixed solvent with low boiling, volatility, polar organic solvent as auxiliary agent and moisture content, be difference, under 30-100 ℃, carry out, if necessary also can stir according to the NMMO moisture;
Among the present invention cellulose pulp mixed with mixed solvent and form an even mixed materials, be to carry out under 30-100 ℃ equally according to not coexisting of NMMO moisture, if necessary also can stir or use in the mixed material device of controllable temperature as be furnished with the vertical or horizontal mixing kettle that the band of chuck and temperature control stirs, the processing time be preferably 30 minutes;
Among the present invention, the low boiling volatile organic solvent is removed from mixed material, be lower than 5% to the content of low boiling volatile organic solvent, be under negative pressure or normal pressure, to carry out, time can be 20-60 minute, and temperature can be adjusted as required, is generally 50-70 ℃.
Among the present invention, mixed material is sent in the dissolution equipment processing be dissolved in NMMO fully, obtain cellulose spinning fluid and can adopt as dissolution kettle until cellulose, equipment such as extruder, temperature can be set at 70-120 ℃.
Among the present invention, described organic solvent can be aliphatic volatility monohydric alcohol, aliphatic volatility monoketone, aliphatic volatility monobasic ether or its mixture.The organic solvent that also can select other for use of the present invention, its addition also can be adjusted as the case may be.Preferred described aliphatic volatility monohydric alcohol is methyl alcohol or ethanol; Described aliphatic volatility monoketone is an acetone.
Among the present invention, preferably the low boiling volatile organic solvent is removed from mixed material, be lower than 1% to the content of low boiling volatile organic solvent.
Among the present invention, from mixed material, remove the method that the low boiling volatile organic solvent can adopt the decompression devolatilization.
Cellulose pulp of the present invention can be a kind of or its mixing in wood pulps, the cotton pulp dregs of rice, bamboo pulp or the hemp dissolving pulp.
After the low boiling point organic solvent removal, can under heating, adopt other dissolution equipments such as single screw extrusion machine, double screw extruder, dissolution kettle that the cellulose in the mixed material is dissolved among the NMMO fully, obtain cellulose spinning fluid.
In an embodiment of the invention, with low boiling, polarity, volatile organic solvent and moisture content is that the NMMO solution of 8-18% mixes the formation mixed solvent, consumption of organic solvent is 0.2-2.0 a times of cellulose pulp weight, be equivalent to that the content of organic solvent is not more than 20% in the mixed solvent, then the raw material pulp is joined in the mixed solvent, mix 40-80 ℃ of stirred in water bath, like this can be so that cellulose pulp mixes with mixed solvent more equably.Recovered under reduced pressure polar organic solvent then, at last mixed material being sent in the dissolution equipment further, dissolving is dissolved in the NMMO solvent fully until cellulose.
Scheme provided by the present invention makes common single screw extrusion machine or double screw extruder become possibility as dissolution equipment, also can adopt other dissolution equipment.
The resulting cellulose spinning fluid of the present invention can be through the spinning machine spinning, and with the moisture content be the NMMO solution of 8-18% as coagulating bath, by solidifying, wash and reeling, obtain regenerated celulose fibre.
The present invention adopts low boiling, polarity, volatile organic solvent, and its acting body is present:
The existence of volatile organic solvent has increased the volume of solvent, can guarantee that solvent mixes with the even of pulp.
Volatile organic solvent is cellulosic non-solvent, will delay cellulosic swelling, stops the too early dissolving of cellulose, makes cellulose dissolution more even.
The adding of volatile organic solvent will reduce the viscosity of solvent, promote the infiltration of solvent to the fibrocyte each several part, improve cellulosic dissolving quality, reduce the content of insoluble particles in the solution.
The volatile organic solvent normal temperature that the present invention uses is liquid down, when cellulose pulp be mixed with after the volatile organic solvent mixed solvent fully mixes, floods, can under normal pressure or vacuum condition, the organic matter auxiliary agent in the mixed material be taken away rapidly to accelerate to remove the process of organic solvent, make the material system enter dissolve area (being equivalent to NMMO moisture content about 13%) very soon, thereby can directly use screw extruder or other dissolution equipment to dissolve, and the recyclable back of organic matter auxiliary agent is reused, and can not cause extra pollution to environment.The present invention need not to dewater after adding pulp, and because the existence of organic solvent, has increased the volume of solvent, has delayed cellulosic swelling, stops the too early dissolving of cellulose, can make cellulose dissolution more evenly, thoroughly.And the adding of volatile organic solvent will reduce the viscosity of solvent, promote the infiltration of solvent to the fibrocyte each several part, improve cellulosic dissolving quality, reduce the content of insoluble particles in the solution.
KR20010093598 adopts and to account for 25% methyl alcohol, ethanol or acetone at least and replace water and mix with NMMO, utilize above organic low specific heat, low boiling to reduce expending of subsequent extracted step, but because the strong absorptive of NMMO be difficult to obtain anhydrous NMMO, thereby its application exists difficulty.And method of the present invention adopts the common NMMO that contains certain crystallization water, and add a small amount of organic solvent to delay cellulosic swelling, stop the too early dissolving of cellulose, reduce the viscosity of solvent, treat to extract organic solvent again after cellulose and mixed solvent mix, complete dissolving cellulos under heating condition, so the present invention at last need not anhydrous NMMO, also can not have the new problem of using anhydrous NMMO to bring.In addition, owing to use methyl alcohol, ethanol or acetone to replace water, the KR20010093598 disclosed method also needs to adopt a large amount of ethanol, methyl alcohol or acetone as coagulating bath, cause production cost to increase, and these three kinds of materials all have volatility, it also can bring new problem as coagulating bath, and the spinning solution that the present invention obtains uses the mixed liquor of traditional NMMO and water as coagulating bath, adopts existing technical equipment and technology to realize.
The present invention is further illustrated below in conjunction with specific embodiment, and described embodiment is used to explain the present invention, and unrestricted the present invention.
The specific embodiment
Embodiment 1
Get moisture content and be 13% NMMO 9 grams, put into the 100ml beaker, place 65-70 ℃ of water-bath, melt fully to solvent, add ethanol 0.7 gram, mix, 1 gram wood pulps (earlier in 80-90 ℃ of baking oven dry 30-40 minute) added constantly stir in the mixed solvent and place 65-70 ℃ of water-bath to place half an hour in beaker, make pulp immerse mixed solvent and evenly mix, then beaker is moved in the vacuum drying oven, vacuumized under 50-70 ℃ 30 minutes, and removed ethanol.Stir material with glass bar at last, and beaker is moved in the 90-100 ℃ of baking oven, material dissolution after 100 minutes is the transparent orange yellow liquid.
Embodiment 2
Get moisture content and be 11% NMMO 8.8 grams, put into the 100ml beaker, place 65-70 ℃ of water-bath, melt fully to solvent, mixture 1.2 grams that add methyl alcohol and ethanol (each 0.6 gram), mix, 1.2 gram bamboo pulps (earlier in 80-90 ℃ of baking oven dry 30-40 minute) are added constantly stir in the mixed solvent and place 65-70 ℃ of water-bath to place half an hour in beaker, make pulp immerse mixed solvent and evenly mixing, then beaker is moved in the vacuum drying oven, vacuumized under 50-70 ℃ 30 minutes, and removed methyl alcohol and ethanol.Stir material with glass bar at last, and beaker is moved in the 90-100 ℃ of baking oven, material dissolution after 150 minutes, solution is transparent, but color is darker slightly than embodiment 1 and embodiment 2.
Embodiment 3
Get moisture content and be 13% NMMO 8.7 grams, put into the 100ml beaker, place 65-70 ℃ of water-bath, melt fully to solvent, add ethanol 1.3 grams, mix, the 1.3 gram cotton pulp dregs of rice (earlier in 80-90 ℃ of baking oven dry 30-40 minute) are added constantly stir in the mixed solvent and place 65-70 ℃ of water-bath to place half an hour in beaker, make pulp immerse mixed solvent and evenly mix, then beaker is moved in the vacuum drying oven, vacuumized under 50-70 ℃ 30 minutes, and removed ethanol.Stir material with glass bar at last, and beaker is moved in the 90-100 ℃ of baking oven, material dissolution after 210 minutes, but solution is dark brown.
Embodiment 4
Get moisture content and be 13% NMMO 9 grams, put into the 100ml beaker, place 65-70 ℃ of water-bath, melt fully to solvent, add acetone 1 gram, mix, 0.5 gram wood pulps and the 0.5 gram cotton pulp dregs of rice (earlier in 80-90 ℃ of baking oven dry 30-40 minute) are added in the mixed solvent and constantly and stir, make pulp immerse mixed solvent and evenly mix, then beaker is moved in the vacuum drying oven, vacuumized under 50-70 ℃ 30 minutes, and removed acetone.Stir material with glass bar at last, and beaker is moved in the 90-100 ℃ of baking oven, material dissolution after 100 minutes is the transparent orange yellow liquid.
Embodiment 5
Get 9 parts of moisture content and be 8% NMMO and dissolve, add 0.36 part of acetone, mix, add 1.8 parts of cotton pulp dregs of rice again, place the mixing kettle that vertical band stirs and chuck heats, stirred 30 minutes 65-70 ℃ of heating; Connection vacuum tube under reduced pressure (50-70 ℃) removal acetone to content of acetone is lower than 5%, then mixed material is sent into dissolution kettle 90-100 ℃ of following heating for dissolving, obtains orange, transparent, thick cellulose solution.Cellulose solution is through the spinning of single unit spinning machine, is that 8% the NMMO-aqueous solution is coagulating bath with moisture content, through solidifying, wash and reeling, obtains regenerated celulose fibre.
Embodiment 6
Get 9 parts of moisture content and be 13% NMMO and dissolve, add 1.3 parts of ethanol, mix, add 1.3 parts of wood pulps again, place the mixing kettle that vertical band stirs and chuck heats, stirred 30 minutes 65-70 ℃ of heating; Connect vacuum tube, decompression (70-80 ℃) removal ethanol to ethanol content down is lower than 1%, then mixed material is sent into twin (double) screw extruder and is added the hot extrusion dissolving, and screw speed is 80-120 rev/min, each Heating Zone Temperature is 80-120 ℃, obtains orange, transparent, thick cellulose solution.Cellulose solution is through the spinning of single unit spinning machine, is that 13% the NMMO-aqueous solution is coagulating bath with moisture content, through solidifying, wash and reeling, obtains regenerated celulose fibre.
Embodiment 7
Get 9 parts of moisture content and be 18% NMMO and dissolve, add 1.8 parts of methyl alcohol, mix, add 0.9 part of bamboo pulp again, place the mixing kettle that vertical band stirs and chuck heats, stirred 30 minutes 65-70 ℃ of heating; Connect vacuum tube down at 70-80 ℃, decompression is removed methyl alcohol to methanol content down and is lower than 3%, then mixed material is sent into single-screw extrusion machine and is added the hot extrusion dissolving, and screw speed is 20-50 rev/min, each Heating Zone Temperature is 70-110 ℃, obtains orange, transparent, thick cellulose solution.Cellulose solution is through the spinning of single unit spinning machine, is that 18% the NMMO-aqueous solution is coagulating bath with moisture content, through solidifying, wash and reeling, obtains regenerated celulose fibre.
Claims (10)
1. the preparation method of a cellulose spinning fluid may further comprise the steps:
(1) be that N-methylmorpholine-N oxide (NMMO) of 8-18% mixes and forms a mixed solvent with low boiling, volatility, polar organic solvent as auxiliary agent and moisture content;
(2) cellulose pulp is mixed formation one even mixed materials with mixed solvent;
(3) the low boiling volatile organic solvent is removed from mixed material, be lower than 5% to the content of low boiling volatile organic solvent.
(4) under heating, make cellulose dissolution in the mixed material in NMMO, obtain cellulose spinning fluid.
2. the preparation method of a kind of cellulose spinning fluid according to claim 1, wherein cellulose pulp is mixed formation one mixed material with mixed solvent after, also comprise the mixed material device that mixed material is placed controllable temperature, and stir even until mixing of materials.
3. the preparation method of a kind of cellulose spinning fluid according to claim 1 is characterized in that, the addition of described cellulose pulp is the 10-20% of the NMMO consumption of moisture content 8-18%.
4. the preparation method of cellulose spinning fluid according to claim 1 is characterized in that, the consumption of mixed solvent Semi-polarity organic solvent is 0.2-2.0 a times of cellulose.
5. according to the preparation method of any one described cellulose spinning fluid of claim 1 to 4, it is characterized in that, described organic solvent is aliphatic volatility monohydric alcohol, aliphatic volatility monoketone, aliphatic volatility monobasic ether or its mixture, and preferred described aliphatic volatility monohydric alcohol is methyl alcohol or ethanol; Described aliphatic volatility monoketone is an acetone.
6. the preparation method of cellulose spinning fluid according to claim 1 is characterized in that, the low boiling volatile organic solvent is removed from mixed material, is lower than 1% to the content of low boiling volatile organic solvent.
7. the preparation method of cellulose spinning fluid according to claim 1 is characterized in that, adopts the method for decompression that the low boiling volatile organic solvent is removed from mixed material.
8. according to the preparation method of any described cellulose spinning fluid of claim 1-4, it is characterized in that described cellulose pulp is a kind of or its mixing in wood pulps, the cotton pulp dregs of rice, bamboo pulp or the hemp dissolving pulp.
9. the preparation method of cellulose spinning fluid according to claim 1 is characterized in that, can adopt single screw extrusion machine, double screw extruder or dissolution kettle to make cellulose dissolution in the mixed material in NMMO, obtains cellulose spinning fluid.
10. the method that the spinning solution that adopts the preparation method of the described cellulose spinning fluid of claim 1 to obtain carries out spinning, it is characterized in that, with the cellulose spinning fluid that obtains through the spinning machine spinning, and be that the NMMO solution of 8-18% is as coagulating bath with the moisture content, by solidifying, wash and reeling, obtain cellulose fibre.
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