CN103668522B - A kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber - Google Patents
A kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber, it is by being added in appropriate amount of deionized water by the micron order calcium silicate powder of particle diameter < 5 μm, ultrasonic disperse, obtained calcium silicates dispersion liquid; Obtained calcium silicates dispersion liquid is added in viscose solution by the 5%-40% of Fire resistant viscose fiber quality and also fully stirs; Follow-up operation process adopts routine techniques means, final obtained Fire resistant viscose fiber product.What play main fire retardation in Fire resistant viscose fiber of the present invention is calcium metal ion.The preparation method of water-insoluble calcium silicates Fire resistant viscose fiber of the present invention, its technique is simple, easy to operate, easy to control, and manufacturing cost relative moderate; Adopt the obtained Fire resistant viscose fiber of the method can reach heat-resisting, flame retardant effect preferably, in use do not discharge toxic gas, after discarded, do not cause environmental pollution.
Description
Technical field
The present invention relates to a kind of preparation method of non-water soluble metal silicate Fire resistant viscose fiber, particularly relate to a kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber.
Background technology
A large amount of construction in high residential building, hotel in recent years and the fast development of the various vehicles have promoted the development of fire resistance fibre technology greatly.Its Application Areas also get home from military, industry, fire-fighting development spin, the ornament materials etc. of the vehicles and public place.Along with the continuous lifting with class that develops rapidly of interior decoration industry, curtain, carpet, fabric decoration etc. have spread to increasing Household fit-up and decoration from the contour shunting yard in hotel already.In recent years, the fire that countries in the world cause because of textiles constantly increases.Show the result that the death by accident caused by fire is investigated, the fire caused by upholstery and textiles holds pride of place.Meanwhile, research finds, the extent of injury of the pernicious gas discharged during flammable textile combustion to human body substantially exceeds flame retardant textiles.Therefore for preventing fire, producing fire resistance fibre and being more and more subject to people's attention.
And the phenomenon of molten drop drippage easily occurs the fire-retardant polyester fibre having realized at present industrialization, the high-temperature fusant that molten drop drippage produces not only can skin ambustion, and the combustible material around that can ignite, and causes more conflagration.And many high temperature posies and have the work position of fire protection requirement to propose great demand to fire resistance fibre, the fire fighter as domestic metallurgical system worker, Coal Mine Staff and substantial amounts has wilderness demand to flame retardant textiles; After Headquarters of the General Staff have several years ago started to equip fire-retardant BDU in army, the demand of following army will be larger.But the mainly fire-retardant polyester fibre of relevant department's equipment, will cause potential injury to relevant user of service at present, the fire-entry suit that fire fighter adopts coating or aramid fiber to produce will be heavy or expensive, can not satisfy the demands completely.
In the development process of flame retarded polymeric material, experienced by initial inorganic salts and the metal oxide of using in the world as material surface process fire retardant, the stage adopting organic halogen based flame retardant, use phosphorus system organic-inorganic fire retardant, organic polymer fire retardant.For halogen, nitrogen, phosphorus type flame retardant, because halogen in use can produce toxic gas, secondary injury is caused to human body, contaminated environment; And although nitrogen, phosphorus fire retardant are non-halogen flame retardant, in process of production, meet fire burning and discarded after also there is the problem of environmental pollution.
Therefore, Green Flammability technology is the trend of fire proofing modification development, represents the development trend of Fire resistant viscose fiber technology.
Chinese patent application CN1635019A discloses a kind of regenerated cellulose/SiO
2the preparation method of nano composite material, it passes through SiO
2nanometer improve SiO
2flame retardant activity, and make Nano-meter SiO_2
2be evenly distributed in regenerated cellulose matrix, make regenerated cellulose/SiO
2nano composite material.It utilizes Nano-meter SiO_2
2flame retardant activity realize the flame-retarded of regenerated cellulose product.
Thisly utilize Nano-meter SiO_2
2flame retardant activity realize the fire-retardant method of regenerated cellulose product, its fire retardant mechanism mainly utilizes Silica hydrogel decomposes to generate water, lowers the temperature by this, and utilizes another catabolite silica to play certain iris action to burning.Above-mentioned this fire retardant mechanism, determines in this Fire resistant viscose fiber product and inevitably there is the too much outstanding problem of inorganic combustion inhibitor addition, and then directly affect the physical property of fiber; And inorganic combustion inhibitor addition is too much, on the one hand, causes a large amount of inorganic combustion inhibitors to be attached to the cortical surface of fiber, to spin or flame retardant effect reduces greatly after making fabric, unstable product quality; On the other hand, a large amount of inorganic combustion inhibitors enters coagulating bath in solidification forming process, brings production line acid bath to reclaim the series of problems such as difficulty, production cost rising.
Summary of the invention
The object of the invention is, provide a kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber, its technique is simple, and easy to operate, the viscose product prepared, when less inorganic combustion inhibitor adds, just can reach heat-resisting, flame retardant effect preferably.
The present invention for achieving the above object technical issues that need to address is, how by dispersed in water for the water-insoluble calcium silicate powder of particle diameter < 5 μm, forms the calcium silicates aqueous dispersions of stable homogeneous; And then micron order silicic acid calcium particle is dispersed in viscose solution, until finally evenly enter and stable existence in viscose.Formed uniform and stable with the technical problem of the Fire resistant viscose fiber of cellulose-calcium silicates composition.
The present invention is the technical scheme solving the problems of the technologies described above employing, and a kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber, is characterized in that, comprise the following steps successively:
Step one, is added in appropriate amount of deionized water by the micron order calcium silicate powder of particle diameter < 5 μm, ultrasonic disperse, obtained calcium silicates dispersion liquid; Wherein, the described ultrasonic disperse time is 5-20 minute;
Step 2, adds in viscose solution by obtained calcium silicates dispersion liquid, fully stirs at 10-40 DEG C; Wherein, the component of described viscose solution by percentage to the quality, is the alpha-cellulose of 6%-9%, the NaOH of 5%-6%, and surplus is water;
The addition of described calcium silicate powder is the 5%-40% of Fire resistant viscose fiber quality;
Step 3, carries out vacuum defoamation process by the mixed solution be uniformly mixed, the gas that removing is wherein contained, forms spinning glue; Wherein, deaeration temperature is 10 DEG C-30 DEG C, and inclined heated plate is 20 minutes-60 minutes;
Step 4, clamp-ons above-mentioned spinning glue and solidifies in acid bath formation spun filament of reeling off raw silk from cocoons, and now, the calcium silicates in spinning glue is bonded in inside and the top layer of spun filament;
Describedly solidify acid bath in one liter, its raw material components is 80 ~ 130 grams, sulfuric acid, 230 ~ 340 grams, sodium sulphate, 0 ~ 20 gram, zinc sulfate, and surplus is water;
Described temperature of solidifying acid bath is 10 DEG C-50 DEG C;
Described spinning glue is 3-10 second in the time of solidifying solidification forming in acid bath;
Step 5, routinely viscose production method, by spun filament successively through multistage drafting, cut-out, washing, alkali cleaning, oil, dry, obtained water-insoluble calcium silicates is as the Fire resistant viscose fiber finished product of fire retardant.
The technique effect that technique scheme is directly brought is, is added in appropriate amount of deionized water, utilizes ultrasonic disperse by the water-insoluble calcium silicate powder of particle diameter < 5 μm, dispersed in water, forms the calcium silicates aqueous dispersions of stable homogeneous; The employing of this technological means, makes water-fast calcium silicates be dispersed in water, forms even, stable calcium silicates dispersion liquid;
And then micron order silicic acid calcium particle is dispersed in viscose solution, acquisition is uniformly dispersed, in stable condition calcium silicates-viscose solution;
Subsequently solidifying solidification forming in acid bath, formed spun filament process in, make the inner homogeneous of spun filament be dispersed with more calcium silicates.That is, micron order silicic acid calcium particle is dispersed in viscose solution, until finally evenly enter also stable existence, in the cellulose of viscose, to form the uniform and stable Fire resistant viscose fiber formed with cellulose-calcium silicates.
Technique scheme, on the one hand, has the technical characterstic that technique is simple, operation and controlling is easy; On the other hand, in the cellulose of viscose, the uniform and stable Fire resistant viscose fiber formed with cellulose-calcium silicates is formed because micron order silicic acid calcium particle finally evenly enters also stable existence.Ensure that more calcium metal ion is dispersed in the inside of spun filament or the stable top layer being embedded in spun filament, significantly decrease the calcium silicates quantity that spun filament top layer exists with " attachment " form; Thus, significantly decrease viscose solution in coagulation bath solidification forming process, a large amount of fire retardant raw material directly enters coagulating bath or is lost in the repeatedly washing, alkaline cleaning procedure of viscose post processing subsequently.
Moreover, on the one hand, the utilization ratio of flame retardant constituent can be improved, reduce consumption; On the other hand, due to significantly raising and the improvement of dispersing uniformity, when ensureing same flame retardant effect, the quantity playing the calcium metal ion of fire retardation that viscose inside is existed can corresponding reduction or minimizing, in brief, the quantity playing the inorganic matter composition of fire retardation in viscose is just reduction of.Like this, the technique effect directly brought is, effectively prevent the excessive loss of the physical indexs such as viscose product strength, improves the quality of final products; In addition, also significantly can reduce the difficulty of the filtration treatment such as the recycling of the water after coagulating bath recovery, post processing, thus indirectly bring the technique effect that viscose manufacturing cost reduces.
For understanding the present invention better, now carry out supplementary comparative illustration with regard to technical scheme disclosed in fire retardant mechanism of the present invention and Chinese patent application CN1635019A: although the flame-retardant additive of the two uses is all silicate, but the technical scheme that CN1635019A adopts joins in viscose glue by water miscible sodium metasilicate or potassium silicate, after entering coagulating bath there is chemical reaction generate polysilicon acid with sour in sodium metasilicate or potassium silicate; Therefore, in the Fire resistant viscose fiber of this patent of invention, what play fire retardation is polysilicon acid.And the present invention's employing is non-water-soluble calcium silicates, after entering coagulating bath, in the fibre, finally, what in Fire resistant viscose fiber, play fire retardation is calcium silicates to the calcium silicates bonding of spun filament inside.In both technical schemes, not no matter the kind of fire retardant, or fire retardant mechanism, be all diverse.
As preferably, the above-mentioned first step comprises: be added to by calcium silicate powder in appropriate amount of deionized water, and ultrasonic wave disperses, obtained calcium silicates dispersion liquid; Wherein, described calcium silicates accounts for the 20%-50% of calcium silicates dispersion liquid gross mass.
The technique effect that this optimal technical scheme is directly brought is, is added in appropriate amount of deionized water, utilizes ultrasonic disperse by the water-insoluble calcium silicate powder of particle diameter < 5 μm, dispersed in water, forms the calcium silicates aqueous dispersions of stable homogeneous; The employing of this technological means, makes water-fast calcium silicates be dispersed in water, forms even, stable calcium silicates dispersion phase.
Further preferably, above-mentioned acid bath temperature of solidifying is 30 DEG C ~ 50 DEG C.
The technique effect that this optimal technical scheme is directly brought is, the reduction of solidification forming temperature can slow down the speed of solidification forming, be conducive to the thorough degree that the alkali in the main component cellulose xanthate ester of viscose solution and the sulfuric acid neutralization reaction in coagulating bath are carried out, namely be conducive to cellulose xanthate ester to be able to Restore All and to become cellulose, and the physical performance index being conducive to final products improving to a certain degree.
Adopt the Fire resistant viscose fiber product that method of the present invention is produced, its fire retardant mechanism is, the calcium metal ion of stable existence between viscose cellulosic molecule gap is utilized to promote under heating status and change the thermal cracking course of cellulosic molecule, decrease the generation of combustible, the pyrolysis of catalyse cellulose molecule becomes more charcoal and water, realizes good flame retardant effect.
In other words, what play main fire retardation in Fire resistant viscose fiber of the present invention is calcium ion, calcium ion has efficient flame retardant effect to cellulose, polysilicon acid is mainly utilized to take away the fire retardant mechanism of heat, dilution combustible and oxygen by thermogenetic water vapor relative to the Fire resistant viscose fiber of prior art, the fire retardant mechanism of the two is completely different, and flame retardant effect difference significantly.
In sum, the preparation method of water-insoluble calcium silicates Fire resistant viscose fiber of the present invention, its beneficial effect is, technique is simple, easy to operate, easy to control, and the manufacturing cost relative moderate of Fire resistant viscose fiber; Adopt the obtained Fire resistant viscose fiber of the method can reach heat-resisting, flame retardant effect preferably.
Detailed description of the invention
Below in conjunction with embodiment, the preparation method to water-insoluble calcium silicates Fire resistant viscose fiber of the present invention is described in detail.
Embodiment 1:
The addition of calcium silicates is 5% of Fire resistant viscose fiber quality;
Sulfuric acid content is 80 grams/L, sodium sulphate 230 grams/L, zinc sulfate 20 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds;
2.2 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 5 minutes, obtained calcium silicates content is the calcium silicates dispersion liquid of 20%, being joined content, to join 500 grams of alpha-cellulose content be 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, abundant stirring 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 80 grams/L, sodium sulphate 230 grams/L, zinc sulfate 20 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 21%.
Embodiment 2:
The addition of calcium silicates is 40% of Fire resistant viscose fiber quality;
Sulfuric acid content is 130 grams/L, sodium sulphate 340 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 10 seconds;
27.83 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 20 minutes, obtained magnesium silicate content is the calcium silicates dispersion liquid of 50%, and being joined 500 grams of alpha-cellulose content is 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, fully stir 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 130 grams/L, sodium sulphate 340 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 10 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 29%.
Embodiment 3:
The addition of calcium silicates is 32.6% of Fire resistant viscose fiber quality;
Sulfuric acid content is 80 grams/L, sodium sulphate 240 grams/L, zinc sulfate 15 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 5 seconds;
20.18 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 20 minutes, obtained calcium silicates content is the calcium silicates dispersion liquid of 50%, and being joined 500 grams of alpha-cellulose content is 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, fully stir 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 80 grams/L, sodium sulphate 240 grams/L, zinc sulfate 15 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 5 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 27%.
Embodiment 4:
The addition of calcium silicates is 25% of Fire resistant viscose fiber quality;
Sulfuric acid content is 100 grams/L, sodium sulphate 240 grams/L, zinc sulfate 15 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 4 seconds;
13.92 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 5 minutes, obtained calcium silicates content is the calcium silicates dispersion liquid of 50%, and being joined 500 grams of alpha-cellulose content is 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, fully stir 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 100 grams/L, sodium sulphate 240 grams/L, zinc sulfate 15 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 4 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 26%.
Embodiment 5:
The addition of calcium silicates is 20% of Fire resistant viscose fiber quality;
Sulfuric acid content is 80 grams/L, sodium sulphate 240 grams/L, zinc sulfate 15 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds;
10.44 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 10 minutes, obtained calcium silicates content is the calcium silicates dispersion liquid of 40%, and being joined 500 grams of alpha-cellulose content is 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, fully stir 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 80 grams/L, sodium sulphate 240 grams/L, zinc sulfate 15 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 25%.
Embodiment 6:
The addition of calcium silicates is 15% of Fire resistant viscose fiber quality;
Sulfuric acid content is 80 grams/L, sodium sulphate 240 grams/L, zinc sulfate 10 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds;
7.37 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 5 minutes, obtained calcium silicates content is the calcium silicates dispersion liquid of 30%, and being joined 500 grams of alpha-cellulose content is 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, fully stir 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 80 grams/L, sodium sulphate 240 grams/L, zinc sulfate 10 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 24%.
Embodiment 7:
The addition of calcium silicates is 10% of Fire resistant viscose fiber quality;
Sulfuric acid content is 80 grams/L, sodium sulphate 300 grams/L, zinc sulfate 15 grams/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds
4.64 grams of calcium silicates are added in appropriate amount of deionized water, ultrasonic disperse 5 minutes, obtained calcium silicates content is the calcium silicates dispersion liquid of 30%, and being joined 500 grams of alpha-cellulose content is 8.35%(quality), sodium hydrate content is 5.8%(quality) viscose solution in, at 10 DEG C-40 DEG C, fully stir 1 hour, be mixed to get viscose glue-calcium silicates dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20 minutes, remove gas contained in dispersion liquid, obtain viscose glue/CaSiO
3blend spinning liquid.By viscose glue/CaSiO
3blend spinning liquid is squeezed into and solidifies in acid bath generation spun filament of reeling off raw silk from cocoons.Wherein, described in solidify acid bath to consist of sulfuric acid content be 80 grams/L, sodium sulphate 300 grams/L, zinc sulfate 15 grams/L, surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 3 seconds.Spun filament through processes such as drawing-off, washing, alkali cleanings, obtains calcium silicates Fire resistant viscose fiber again.Recording limited oxygen index is 23%.
Claims (3)
1. a preparation method for water-insoluble calcium silicates Fire resistant viscose fiber, is characterized in that, comprise the following steps successively:
Step one, is added in appropriate amount of deionized water by the micron order calcium silicate powder of particle diameter < 5 μm, ultrasonic disperse, obtained calcium silicates dispersion liquid; Wherein, the described ultrasonic disperse time is 5-20 minute;
Step 2, adds in viscose solution by calcium silicates dispersion liquid obtained in step one, fully stirs at 10-40 DEG C; Wherein, described viscose solution by percentage to the quality, comprises the alpha-cellulose that mass percent is 6%-9%, the NaOH of 5%-6%, and surplus is water;
The addition of described calcium silicates is the 5%-40% of Fire resistant viscose fiber quality;
Step 3, carries out vacuum defoamation process to remove gas contained in solution, forms spinning glue by the mixed solution of step 2 after stirring; Wherein, deaeration temperature is 10 DEG C-30 DEG C, and inclined heated plate is 20 minutes-60 minutes;
Step 4, clamp-oned by the spinning glue of the formation in step 3 and solidify in acid bath formation spun filament of reeling off raw silk from cocoons, calcium silicates is dispersed in inside and the top layer of spun filament;
Describedly solidify acid bath in one liter, its raw material components is 80 ~ 130 grams, sulfuric acid, 230 ~ 340 grams, sodium sulphate, 0 ~ 20 gram, zinc sulfate, and surplus is water;
Described temperature of solidifying acid bath is 10 DEG C-50 DEG C;
Described spinning glue is 3-10 second in the time of solidifying solidification forming in acid bath;
Step 5, routinely viscose production method, by spun filament successively through multistage drafting, cut-out, washing, alkali cleaning, oil, dry, obtained water-insoluble calcium silicates is as the Fire resistant viscose fiber finished product of fire retardant.
2. the preparation method of water-insoluble calcium silicates Fire resistant viscose fiber according to claim 1, is characterized in that, in above-mentioned steps one, described calcium silicate powder accounts for the 20%-50% of described calcium silicates dispersion liquid gross mass.
3. the preparation method of water-insoluble calcium silicates Fire resistant viscose fiber according to claim 1 and 2, is characterized in that, described in solidify acid bath temperature be preferably 30 DEG C ~ 50 DEG C.
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| EP1918431A1 (en) * | 2005-08-26 | 2008-05-07 | Daiwabo Co. Ltd. | Flameproof rayon fiber and process for production thereof |
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