CN103696030B - A kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber - Google Patents
A kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber Download PDFInfo
- Publication number
- CN103696030B CN103696030B CN201310681905.5A CN201310681905A CN103696030B CN 103696030 B CN103696030 B CN 103696030B CN 201310681905 A CN201310681905 A CN 201310681905A CN 103696030 B CN103696030 B CN 103696030B
- Authority
- CN
- China
- Prior art keywords
- zirconium silicate
- fire
- water
- viscose fiber
- resistant viscose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber, it is by being added in appropriate amount of deionized water by the micron order zirconium silicate powder of particle diameter < 5 μm, ultrasonic disperse, obtained zirconium silicate dispersion liquid; Obtained zirconium silicate 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 metal zirconium ion.The preparation method of water-insoluble zirconium silicate 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 zirconium silicate 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 zirconium silicate 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 particle diameter < 5 μm water-insoluble zirconium silicate powder dispersed in water, form the zirconium silicate aqueous dispersions of stable homogeneous; And then micron order zirconium silicate uniform 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-zirconium silicate composition.
The present invention is the technical scheme solving the problems of the technologies described above employing is that a kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber, is characterized in that, comprises the following steps successively:
Step one, is added in appropriate amount of deionized water by the micron order zirconium silicate powder of particle diameter < 5 μm, ultrasonic disperse, obtained zirconium silicate dispersion liquid; Wherein, the described ultrasonic disperse time is 5-20 minute;
Step 2, adds in viscose solution by obtained zirconium silicate 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 zirconium 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 zirconium silicate 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 zirconium silicate 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 zirconium silicate powder of particle diameter < 5 μm, dispersed in water, forms the zirconium silicate aqueous dispersions of stable homogeneous; The employing of this technological means, makes water-fast zirconium silicate be dispersed in water, forms even, stable zirconium silicate dispersion liquid;
And then micron order zirconium silicate uniform particle is dispersed in viscose solution, acquisition is uniformly dispersed, in stable condition zirconium silicate-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 zirconium silicate.That is, micron order zirconium silicate uniform 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-zirconium silicate.
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-zirconium silicate is formed because micron order zirconium silicate particle finally evenly enters also stable existence.Ensure that more metal zirconium ion is dispersed in the inside of spun filament or the stable top layer being embedded in spun filament, significantly decrease the zirconium silicate 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 metal zirconium 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 zirconium silicate, after entering coagulating bath, in the fibre, finally, what in Fire resistant viscose fiber, play fire retardation is zirconium silicate to the zirconium silicate 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 zirconium silicate powder in appropriate amount of deionized water, and ultrasonic wave disperses, obtained zirconium silicate dispersion liquid; Wherein, described zirconium silicate accounts for the 20%-50% of zirconium silicate 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 zirconium silicate powder of particle diameter < 5 μm, dispersed in water, forms the zirconium silicate aqueous dispersions of stable homogeneous; The employing of this technological means, makes water-fast zirconium silicate be dispersed in water, forms even, stable zirconium silicate 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.
For understanding the present invention better, be now further described in conjunction with fire retardant mechanism.Adopt the Fire resistant viscose fiber product that method of the present invention is produced, its fire retardant mechanism is, the metal zirconium 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 zirconium ion, zirconium 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 zirconium silicate 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 zirconium silicate fire-resistant viscose fiber of the present invention is described in detail.
Embodiment 1:
The addition of zirconium silicate is 5% of Fire resistant viscose fiber;
Sulfuric acid content is 80g/L, sodium sulphate 230g/L, zinc sulfate 20g/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 zirconium silicates are added in appropriate amount of deionized water, ultrasonic disperse 5min, obtained zirconium silicate content is the zirconium silicate 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-zirconium silicate dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20min, remove gas contained in dispersion liquid, obtain viscose glue/ZrSiO
4blend spinning liquid.By viscose glue/ZrSiO
4blend 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 80g/L, sodium sulphate 230g/L, zinc sulfate 20g/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 zirconium silicate Fire resistant viscose fiber again.Recording limited oxygen index is 21%.
Embodiment 2:
The addition of zirconium silicate is 40% of Fire resistant viscose fiber;
Sulfuric acid content is 130g/L, sodium sulphate 340g/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 zirconium silicates are added in appropriate amount of deionized water, ultrasonic disperse 20min, obtained magnesium silicate content is the zirconium silicate 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-zirconium silicate dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20min, remove gas contained in dispersion liquid, obtain viscose glue/ZrSiO
4blend spinning liquid.By viscose glue/ZrSiO
4blend 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 130g/L, sodium sulphate 340g/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 zirconium silicate Fire resistant viscose fiber again.Recording limited oxygen index is 30%.
Embodiment 3:
The addition of zirconium silicate is 25% of Fire resistant viscose fiber;
Sulfuric acid content is 80g/L, sodium sulphate 240g/L, zinc sulfate 15g/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 5 seconds;
13.92 grams of zirconium silicates are added in appropriate amount of deionized water, ultrasonic disperse 15min, obtained zirconium silicate content is the zirconium silicate 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-zirconium silicate dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20min, remove gas contained in dispersion liquid, obtain viscose glue/ZrSiO
4blend spinning liquid.By viscose glue/ZrSiO
4blend 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 80g/L, sodium sulphate 240g/L, zinc sulfate 15g/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 zirconium silicate Fire resistant viscose fiber again.Recording limited oxygen index is 27%.
Embodiment 4:
The addition of zirconium silicate is 20% of Fire resistant viscose fiber;
Sulfuric acid content is 100g/L, sodium sulphate 240g/L, zinc sulfate 15g/L, and surplus is water; Solidifying acid bath temperature is 10 DEG C-50 DEG C, and setting time is 4 seconds;
10.44 grams of zirconium silicates are added in appropriate amount of deionized water, ultrasonic disperse 10min, obtained zirconium silicate content is the zirconium silicate 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-zirconium silicate dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20min, remove gas contained in dispersion liquid, obtain viscose glue/ZrSiO
4blend spinning liquid.By viscose glue/ZrSiO
4blend 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 100g/L, sodium sulphate 240g/L, zinc sulfate 15g/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 zirconium silicate Fire resistant viscose fiber again.Recording limited oxygen index is 26%.
Embodiment 5:
The addition of zirconium silicate is 10% of Fire resistant viscose fiber;
Sulfuric acid content is 80g/L, sodium sulphate 240g/L, zinc sulfate 15g/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 zirconium silicates are added in appropriate amount of deionized water, ultrasonic disperse 5min, obtained zirconium silicate content is the zirconium silicate 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-zirconium silicate dispersion liquid, then at 10 DEG C-30 DEG C, carry out vacuum defoamation process 20min, remove gas contained in dispersion liquid, obtain viscose glue/ZrSiO
4blend spinning liquid.By viscose glue/ZrSiO
4blend 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 80g/L, sodium sulphate 240g/L, zinc sulfate 15g/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 zirconium silicate Fire resistant viscose fiber again.Recording limited oxygen index is 26%.
Claims (3)
1. a preparation method for water-insoluble zirconium silicate fire-resistant viscose fiber, is characterized in that, comprises the following steps successively:
Step one, is added in appropriate amount of deionized water by the micron order zirconium silicate powder of particle diameter < 5 μm, ultrasonic disperse, obtained zirconium silicate dispersion liquid; Wherein, the described ultrasonic disperse time is 5-20 minute;
Step 2, adds in viscose solution by zirconium silicate 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 zirconium silicate 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, zirconium silicate 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 zirconium silicate is as the Fire resistant viscose fiber finished product of fire retardant.
2. the preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber according to claim 1, is characterized in that, in above-mentioned steps one, described zirconium silicate powder accounts for the 20%-50% of described zirconium silicate dispersion liquid gross mass.
3. the preparation method of water-insoluble zirconium silicate 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310681905.5A CN103696030B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310681905.5A CN103696030B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103696030A CN103696030A (en) | 2014-04-02 |
| CN103696030B true CN103696030B (en) | 2015-09-02 |
Family
ID=50357686
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310681905.5A Active CN103696030B (en) | 2013-12-12 | 2013-12-12 | A kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103696030B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800248A (en) * | 2005-01-07 | 2006-07-12 | 青岛大学 | Preparation method of regenerated cellulose / nanometer SiO2 fire-retardant composite material |
| CN101050559A (en) * | 2006-04-09 | 2007-10-10 | 青岛大学 | Method for preparing Nano SiO2 fire retardant viscose fiber, and film |
| CN102352539A (en) * | 2011-07-27 | 2012-02-15 | 杭州奥通特种纤维技术有限公司 | Manufacturing method of silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber |
| CN102505169A (en) * | 2011-10-26 | 2012-06-20 | 阜宁澳洋科技有限责任公司 | Flame-retardant viscose fiber and preparation method thereof |
-
2013
- 2013-12-12 CN CN201310681905.5A patent/CN103696030B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1800248A (en) * | 2005-01-07 | 2006-07-12 | 青岛大学 | Preparation method of regenerated cellulose / nanometer SiO2 fire-retardant composite material |
| CN101050559A (en) * | 2006-04-09 | 2007-10-10 | 青岛大学 | Method for preparing Nano SiO2 fire retardant viscose fiber, and film |
| CN102352539A (en) * | 2011-07-27 | 2012-02-15 | 杭州奥通特种纤维技术有限公司 | Manufacturing method of silicon-nitrogen containing environmental protection and flame retardant viscose staple fiber |
| CN102505169A (en) * | 2011-10-26 | 2012-06-20 | 阜宁澳洋科技有限责任公司 | Flame-retardant viscose fiber and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 《阻燃粘胶纤维的制备及性能研究》;全凤玉;《中国优秀硕士学位论文全文数据库工程科技I辑》;20040315;第三章第37页，第六章第70页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103696030A (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8133583B2 (en) | Fire retardant antiflux fiber and its production process | |
| CN106521691B (en) | Polyester fiber with flame-proof antibiotic characteristic and its application | |
| CN101215726A (en) | Method for preparing flame-proof viscose fiber | |
| CN100465359C (en) | Technological process of producing fire retardant antiflux fiber | |
| CN103668521B (en) | A kind of preparation method of water-insoluble magnesium silicate Fire resistant viscose fiber | |
| WO2008098518A1 (en) | The flame retardant treatment method for light natural fiber material | |
| CN102286799A (en) | Fire-retardant viscose fiber and preparation method thereof | |
| CN102031583A (en) | Method for manufacturing nano inorganic flame-retardant polyester fibers | |
| CN113584622B (en) | Preparation method of multifunctional environment-friendly flame-retardant wall fabric | |
| CN109019616A (en) | A kind of preparation and application of silica/molybdenum disulfide three-dimensional hybrid material | |
| CN114318589B (en) | High-flame-retardance superfine sea-island yarn and preparation process thereof | |
| CN101914849A (en) | Aluminum hydroxide sol-coated high-temperature-resistant fiber fabric and preparation method thereof | |
| CN113463209B (en) | Flame retardant, and preparation method and application thereof | |
| CN103668522B (en) | A kind of preparation method of water-insoluble calcium silicates Fire resistant viscose fiber | |
| CN102965750B (en) | Method for preparing flame retardant viscose fiber | |
| CN110978683A (en) | High-temperature-resistant double-layer metal melting splashing-preventing fabric and processing technology thereof | |
| CN103696030B (en) | A kind of preparation method of water-insoluble zirconium silicate fire-resistant viscose fiber | |
| CN103696029B (en) | A kind of preparation method of water-insoluble alumina silicate Fire resistant viscose fiber | |
| CN106087101A (en) | A kind of fire-resistant antistatic polyester fiber | |
| CN103643334B (en) | The preparation method of Fire resistant viscose fiber | |
| CN105624825B (en) | A kind of fire-retardant melt-blown non-woven material and preparation method thereof | |
| CN105986474A (en) | High temperature-resistant flame retardation polyacrylonitrile fiber and production method thereof | |
| CN111910281A (en) | Environment-friendly flame-retardant viscose fiber and preparation method thereof | |
| CN113802212B (en) | Flame-retardant fiber, preparation method thereof and flame-retardant fabric | |
| CN1540047A (en) | Method for producing Nano fire resistant and fire retardant fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |