CN102286799A - Fire-retardant viscose fiber and preparation method thereof - Google Patents
Fire-retardant viscose fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a fire-retardant viscose fiber and a preparation method thereof, wherein a silicon and aluminum composite fire retardant is contained in the fire-retardant viscose fiber and the preparation method of the fire-retardant fiber comprises the steps of: obtaining a spinning solution through taking cellulose pulps as a raw material and subjecting to the processing steps of yellowing, dissolving, defoaming and filtering, subjecting the spinning solution to spinning and forming in a coagulating bath, subjecting to post-processing steps of washing and desulfurization, adding right amount of sodium metasilicate and sodium metasilicate solution into a cellulose viscose solution which is dissolved to any process before the spinning and then uniformly mixing. According to the invention, the silicon and aluminum composite fire retardant is utilized to ensure that the fire-retardant effect of the prepared fire-retardant viscose fiber is greatly increased and the high temperature and alkaline resistances of the fire-retardant viscose are greatly increased; and therefore, the fire-retardant viscose fiber can be popularized and applied in high-temperature environments such as the fields of high-temperature filter media, filter materials and the like.
Description
Technical field
The present invention relates to Fire resistant viscose fiber, relate in particular to a kind of with silicon, aluminium as Fire resistant viscose fiber of composite flame-retardant agent and preparation method thereof.
Background technology
Along with the raising of living standards of the people and the enhancing of the security protection consciousness that people-oriented, the fire resistance of fibre more and more is subjected to people's attention.Had a lot of countries and regions to formulate product standard, some fibre of uses such as the regulation vehicles, public place, old man, children must possess fire resistance.Along with the development of fire resistance fibre technology, further require fire resistance fibre in environmental protection, heatproof, be beneficial to aspects such as weaving processing, comfortableness more performance arranged, to satisfy demands of social development.
The flame-retardant modified main use phosphoric acid ester organic fire-retardant and the silicates inorganic combustion inhibitor of at present domestic and international regenerated celulose fibre, the representative products of the fire-retardant regenerated celulose fibre of suitability for industrialized production, the one, the Viscosa FR Fire resistant viscose fiber of Austrian lenzing company, also there is small lot batch manufacture in companies such as domestic Jilin chemical fibre, Tangshan three friends, all are the phosphoric acid based flame retardants that add phosphorous, nitrogen, sulphur ignition-proof element before spinning in the stoste; This fire retardant mainly is a pyrophosphate class organic compound, and ignition-proof element is a p and s, is fire-retardant dose of a kind of interpolation blending type that effectively is used for viscose, and the limited oxygen index of its Fire resistant viscose fiber is greater than 27, and better spinnability is arranged.The 2nd, the Visil series composite flame-proof viscose that the Kemira Co.,Ltd of Finland (Kemira) produces, it mainly is the Visil fiber that contains poly-silicic acid, sea otter also has exploitation in domestic Shandong, the Visil Fire resistant viscose fiber has higher high temperature resistant and flame retardant effect, when burning, toxic gas be can not produce again simultaneously, a spot of smog, CO and CO only produced
2Gas.
But the shortcoming of above-mentioned two kinds of fire-retardant regenerated celulose fibres is, the former emits a large amount of poisonous dense smokes when fiber burns, environment protecting is poor, and the people is suffocated, and the fire retardant cost is very high, product is mainly used in extraordinary fields such as army, fire-fighting, and it is big to apply difficulty at civil area, and its development prospect is also pessimistic; It is the weaving processing difficulties that there is subject matter in the latter, and alkaline resistance properties is poor, is mainly used in fabrics for industrial use, in the field of textiles application difficult, its high temperature resistant disposal ability is also relatively poor simultaneously, is difficult at high temperature, apply as fields such as high temperature filter material, filtrates, have bigger limitation.
Summary of the invention
First technical problem to be solved by this invention is: the deficiency at prior art exists provides a kind of good flame retardation effect and Fire resistant viscose fiber high temperature resistant, that alkaline resistance properties is good.
Second technical problem to be solved by this invention is: at the deficiency that prior art exists, provide the preparation method of a kind of good flame retardation effect and high temperature resistant, that alkaline resistance properties is good Fire resistant viscose fiber.
For solving above-mentioned first technical problem, technical scheme of the present invention is:
A kind of Fire resistant viscose fiber contains silicon, aluminium composite flame-retardant agent in the described Fire resistant viscose fiber.
Preferably, described Fire resistant viscose fiber mainly is made up of by following weight portion silicon, aluminium and cellulose:
Silicon is (with SiO
2Meter) 20～40 part
Aluminium is (with Al
2O
3Meter) 0.5～10 part
50～65 parts of celluloses.
For solving above-mentioned second technical problem, technical scheme of the present invention is:
With the cellulose pulp is raw material, comprise that yellow, dissolving, deaeration and filtration step make spinning solution, with spinning solution spinning moulding in coagulating bath, again through the washing, desulfurization post-processing step, in the cellulose viscose solution of described arbitrary operation before being dissolved to spinning, add an amount of sodium metasilicate and sodium aluminate solution, and mix.
As a kind of preferred, with SiO
2Meter, the addition of sodium metasilicate are 40～60wt% of the fine weight of first in the viscose glue; With Al
2O
3Meter, the addition of sodium metaaluminate are 0.8～15wt% of the fine weight of first in the viscose glue.
Described coagulating bath consist of sulfuric acid 100～150g/L, zinc sulfate 5～50g/L, sodium sulphate 250～350g/L, the acid bath temperature is 30～60 ℃.
As a kind of improvement, the desulfurizing agent during described desulfurization is a sodium sulfite.
As a kind of preferred, the modulus of described sodium metasilicate is 1～4.5, and the modulus of sodium metasilicate can be divided into high, medium and low three kinds, can do different choice according to different hybrid techniques.
The conventional preparation technology of cellulose viscose glue, as those skilled in the art are technique known problems, with the cellulose pulp is raw material, through dipping, squeezing, pulverizing, experienced, yellow, dissolving, filtration, maturation, deaeration, spinning, plasticizing drawing-off, cut off, comprise steps preparations such as washing, desulfurization, the refining of going up wet goods, oven dry.Wherein, in cellulose viscose glue preparation process, the composition of viscose glue may be controlled to alpha-cellulose content 7～10%, and alkali content (in NaOH) 4～7%, viscose riscosity may be controlled to 30～80s (falling ball method).
Among the present invention, sodium metasilicate, sodium aluminate solution join in the cellulose viscose glue and can the arbitrary operation before being dissolved to spinning implement, for example: the one, finish the back in the yellow of cellulose viscose glue and together add with dissolving water, after sodium metasilicate, sodium aluminate solution and viscose glue mix, after filtration, operation such as deaeration, maturation, enter spinning.The 2nd, before rayon spinning, inject through syringe pump, by mode static, dynamic or that the sound attitude is mixed, reach the purpose that mixes with viscose glue, after viscose glue mixes, enter spinning process immediately.In addition, also can filter the back as II F and add in other links in the cellulose viscose glue preparation process.
Owing to adopted technique scheme, the invention has the beneficial effects as follows:
1, the present invention adopts sodium metasilicate and sodium metaaluminate as fire retardant, because sodium metasilicate, the aqueous solution of sodium metaaluminate all is alkalescence, identical with the cellulose viscose glue of alkalescence, so the three has compatibility preferably, sodium metasilicate, sodium metaaluminate and cellulose viscose glue three's mixed solution, enter sulfur acid, zinc sulfate, after the coagulating bath of sodium sulphate, sodium metasilicate is under the effect of sulfuric acid, aggregate into the poly-silicic acid of certain degree of polymerization, sodium metaaluminate and effect of sulfuric acid, generate aluminium hydroxide rapidly, aluminium hydroxide is a kind of the nontoxic of environmental safety and safety in utilization that have, non-harmful inorganic combustion inhibitor, a kind of inorganic combustion inhibitor of the amount of being to use maximum, be called nuisanceless fire retardant by reputation abroad, at plastics, rubber flame-retarded field is used very extensive, its fire retardant mechanism is to contain the hydroxyl that can generate water in the aluminium hydroxide fire retardant, the aluminium hydroxide decomposition temperature is 200 ℃, it finishes dehydration basically in 245～300 ℃ of scopes, discharge the crystallization water, absorb latent heat, reduce temperature, decomposes is emitted a large amount of steam, it is strong endothermic reaction, play the effect of cooling polymer, the steam that reaction produces can dilute the polymerization fuel gas, suppressing burning spreads, newly-generated aluminium oxide also has higher activity, can adsorb soot dust granule, play and press down the cigarette effect, and generate the good equally distributed metal oxide of fire resistance on the combustible surface behind the aluminium hydroxide dehydration, can form fine and close fire-retardant barrier together with other carbide, secluding air, reduce burn rate, thereby reduced the mass loss rate of catabolite, prevent propagation of flame.Therefore, the present invention is through the compound action of silicon, aluminium, the flame retardant effect of Fire resistant viscose fiber improves greatly, the high temperature sintering level of residue of Fire resistant viscose fiber significantly improves when using poly-silicic acid separately, and following table is the Fire resistant viscose fiber of the present invention's preparation ignition residue content when 800 ℃, the addition of gathering silicic acid are the 50wt% of first fibre:
| Aluminium to the addition of first fibre (with Al 2O 3Meter) | Fiber number (dtex) | Ash (wt%) |
| 0(is to the fine wt% of first) | 3.44 | 29.47 |
| 2.3(to the fine wt% of first) | 3.24 | 33.26 |
| 4.6(to the fine wt% of first) | 3.17 | 32.09 |
| 6.9(to the fine wt% of first) | 3.10 | 31.31 |
As can be seen from the above table, only add a spot of aluminium salt, the ignition residue of Fire resistant viscose fiber just is significantly improved, and the experiment of being done under the situation of other ignition temperatures and poly-silicic acid addition all presents identical rule.
2, the present invention adopts silicon, aluminium composite flame-retardant agent, and the resistance to elevated temperatures of the fire resistance fibre that makes significantly improves.This be since on the one hand the mixed solution of aluminium salt and sodium metasilicate and cellulose viscose glue in coagulating bath, the chemical bonding effect can take place, aluminium ion enters the network structure and the effect of poly-silicic acid generation chemical bonding of poly-silicic acid, diaspore disappears, gather aluminosilicate and form, the heat-resisting quantity of poly-aluminosilicate is far above poly-silicic acid, poly-on the other hand aluminosilicate and silicon, aluminium is created in the cellulose macromolecule with the net distribution structure, with the molecular link strong bonded, improved the resistance to elevated temperatures of fire resistance fibre, near the inflammable phenomenon that can significantly suppress cellulose to be decomposed into gas 340 ℃ and cause takes place, and oxygen reaches the purpose that stops burning with contacting of cellulosic matrix thereby its fire retardant mechanism is mainly formation carbon-coating obstruction.The Fire resistant viscose fiber of the present invention preparation when burning, a fiber carbon elementization, not fusion, even carry out continuous burning more than the 3h in 800 ℃ of high temperature, the network structure of fire retardant in fiber is still constant.
3, the fire retardant sodium metasilicate that uses among the present invention, sodium aluminate and cellulose viscose glue all are basoids, so the three has compatibility preferably, the stable filtration and the spinning properties that has guaranteed spinning solution in the Fire resistant viscose fiber preparation process of colloidal dispersion, make the Fire resistant viscose fiber stable production process, technology is controlled easily; And in cellulose viscose glue moulding in coagulating bath the becoming cellulose macromolecule chain structure, silicon, aluminium are created in the cellulose macromolecule with the net distribution structure, with the molecular link strong bonded, improved the alkali resistance of fiber, help Fire resistant viscose fiber spinning, weave the process stabilizing with process.
4, the present invention adopts sodium sulfite as desulfurizing agent in the desulfurization process of post-processing step, has prevented that conventional viscose from adopting the destruction of NaOH desulfurization to poly-silicic acid, aluminium hydroxide flame-retardant composition in producing, and guaranteed flame retardant effect.
5, the present invention is main raw material(s) with the native cellulose, raw material are renewable, but the discarded object natural degradation, and the fire retardant silicon, the aluminium that adopt all are nuisanceless fire retardants, environment is not produced pollution, thereby Fire resistant viscose fiber of the present invention is a kind of environmental protection fiber.
The specific embodiment
Further set forth the present invention below in conjunction with specific embodiment.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 12.22dtex * 51mm Fire resistant viscose fiber
With the cotton pulp dregs of rice is raw material, makes the 5kg alkali cellulose through dipping, squeezing, pulverizing, processing step such as experienced, contains alkali 16.5% in the alkali cellulose, and alpha-cellulose 30.5% is with sodium metasilicate (Na
2SiO
35H
2O) 3.0kg and sodium metaaluminate (NaAlO
2) 0.05kg joins in the 12L soft water fully dissolving, and join in the sodium cellulose xanghate after the alkali cellulose yellow, with the sodium cellulose xanghate mixed dissolution be the fire-retardant cellulose viscose glue, in coagulating bath, carry out spinning behind maturation after filtration,, deaeration, the filtration step, sulfuric acid concentration is 105g/L in the coagulating bath, zinc sulfate concentration is 30g/L, sodium sulfate concentration is 280g/L, temperature is 45 ℃, again through plastifying drawing-off, cut-out, washing, the desulfurization of use sodium sulfite desulfurizing agent, oiling, dry and prepare 2.22dtex * 51mm Fire resistant viscose fiber.
Embodiment 21.67dtex * 38mm Fire resistant viscose fiber
With the wood pulps is raw material, makes the 5kg alkali cellulose through dipping, squeezing, pulverizing, processing step such as experienced, contains alkali 16.5% in the alkali cellulose, and alpha-cellulose 30.3% is with sodium metasilicate (Na
2SiO
39H
2O) 3.3kg and sodium metaaluminate (NaAlO
2) 0.10kg joins in the 12L soft water fully dissolving, and join in the sodium cellulose xanghate after the alkali cellulose yellow, with the sodium cellulose xanghate mixed dissolution be the fire-retardant cellulose viscose glue, in coagulating bath, carry out spinning behind maturation after filtration,, deaeration, the filtration step, sulfuric acid concentration is 145g/L in the coagulating bath, zinc sulfate concentration is 50g/L, sodium sulfate concentration is 350g/L, temperature is 58 ℃, again through plastifying drawing-off, cut-out, washing, the desulfurization of use sodium sulfite desulfurizing agent, oiling, dry and prepare 1.67dtex * 38mm Fire resistant viscose fiber.
Embodiment 33.33dtex * 60mm Fire resistant viscose fiber
With the cotton pulp dregs of rice is raw material, makes 30L cellulose viscose glue through steps such as dipping, squeezing, pulverizing, experienced, chrysanthemum, dissolving, filtration, maturation, deaerations, contains alkali 4.5% in the cellulose viscose glue, and alpha-cellulose 9.1% is 2 sodium metasilicate (Na with modulus
2SiO
35H
2O) 5.0kg and sodium metaaluminate (NaAlO
2) 0.30kg joins in the 2.7L soft water fully dissolving, join in the ducted cellulose viscose glue of viscose glue before the spinning with syringe pump, by static and dynamic mixer cellulose viscose glue and fire retardant are mixed then and make the fire-retardant cellulose viscose glue, in coagulating bath, carry out spinning, sulfuric acid concentration is 115g/L in the coagulating bath, zinc sulfate concentration is 40g/L, sodium sulfate concentration is 300g/L, temperature is 54 ℃, again through plastifying drawing-off, cut-out, washing, the desulfurization of use sodium sulfite desulfurizing agent, oiling, dry and prepare 3.33dtex * 60mm Fire resistant viscose fiber.
Embodiment 43.33dtex * 60mm Fire resistant viscose fiber
With the 30% cotton pulp dregs of rice and 70% wood pulps is raw material, make 30L cellulose viscose glue through steps such as dipping, squeezing, pulverizing, experienced, chrysanthemum, dissolving, filtration, maturation, deaerations, contain alkali 4.7% in the cellulose viscose glue, alpha-cellulose 9.5% is 3.5 sodium metasilicate (Na with modulus
2SiO
35H
2O) 4.5kg and sodium metaaluminate (NaAlO
2) 0.35kg joins in the 3.0L soft water fully dissolving, join in the ducted cellulose viscose glue of viscose glue before the spinning with syringe pump, by static and dynamic mixer cellulose viscose glue and fire retardant are mixed then and make the fire-retardant cellulose viscose glue, in coagulating bath, carry out spinning, sulfuric acid concentration is 125g/L in the coagulating bath, zinc sulfate concentration is 45g/L, sodium sulfate concentration is 320g/L, temperature is 51 ℃, again through plastifying drawing-off, cut-out, washing, the desulfurization of use sodium sulfite desulfurizing agent, oiling, dry and prepare 3.33dtex * 60mm Fire resistant viscose fiber.
Claims (7)
1. a Fire resistant viscose fiber is characterized in that: contain silicon, aluminium composite flame-retardant agent in the described Fire resistant viscose fiber.
2. Fire resistant viscose fiber as claimed in claim 1 is characterized in that: described Fire resistant viscose fiber mainly is made up of by following weight portion silicon, aluminium and cellulose:
Silicon is (with SiO
2Meter) 20～40 part
Aluminium is (with Al
2O
3Meter) 0.5～10 part
50～65 parts of celluloses.
3. the method for preparing Fire resistant viscose fiber as claimed in claim 1, with the cellulose pulp is raw material, comprise that yellow, dissolving, deaeration and filtration step make spinning solution, with spinning solution spinning moulding in coagulating bath, again through the washing, desulfurization post-processing step, it is characterized in that: in the cellulose viscose solution of described arbitrary operation before being dissolved to spinning, add an amount of sodium metasilicate and sodium aluminate solution, and mix.
4. the preparation method of Fire resistant viscose fiber as claimed in claim 3 is characterized in that: with SiO
2Meter, the addition of sodium metasilicate are 40～60wt% of the fine weight of first in the viscose glue; With Al
2O
3Meter, the addition of sodium metaaluminate are 0.8～15wt% of the fine weight of first in the viscose glue.
5. the preparation method of Fire resistant viscose fiber as claimed in claim 4 is characterized in that: described coagulating bath consist of sulfuric acid 100～150g/L, zinc sulfate 5～50g/L, sodium sulphate 250～350g/L, the acid bath temperature is 30～60 ℃.
6. as the preparation method of claim 3,4 or 5 described Fire resistant viscose fiber, it is characterized in that: the desulfurizing agent during described desulfurization is a sodium sulfite.
7. the preparation method of Fire resistant viscose fiber as claimed in claim 6, it is characterized in that: the modulus of described sodium metasilicate is 1～4.5.
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Cited By (8)
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| CN103643335A (en) * | 2013-12-17 | 2014-03-19 | 青岛大学 | Preparation method of flame-retardant viscose fiber |
| CN104233803A (en) * | 2014-09-19 | 2014-12-24 | 太仓苏纶纺织化纤有限公司 | Dip coating preparation method of modified basalt fiber/polyphenylene sulfide composite filter material |
| CN108035004A (en) * | 2017-11-20 | 2018-05-15 | 河北吉藁化纤有限责任公司 | A kind of flame retardant viscose fiber and preparation method thereof |
| CN108677351A (en) * | 2018-05-18 | 2018-10-19 | 宁波荣昌祥服饰股份有限公司 | A kind of anti-bacterial and anti-fouling shirt fabric |
| CN109137112A (en) * | 2018-08-03 | 2019-01-04 | 江南大学 | A kind of fire resistance fibre for automobile interiors and preparation method thereof |
| CN111041567A (en) * | 2019-12-19 | 2020-04-21 | 阜宁澳洋科技有限责任公司 | Method for manufacturing aluminum-containing viscose fibers |
| CN112048827A (en) * | 2020-09-11 | 2020-12-08 | 秦小康 | Melt-blown short fiber spinning method and non-woven fabric filter material product prepared by same |
| CN113293449A (en) * | 2021-07-27 | 2021-08-24 | 兴晔新材料(南通)有限公司 | Preparation method of high-temperature-resistant artificial fiber |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643335A (en) * | 2013-12-17 | 2014-03-19 | 青岛大学 | Preparation method of flame-retardant viscose fiber |
| CN103643335B (en) * | 2013-12-17 | 2016-04-06 | 青岛大学 | The preparation method of Fire resistant viscose fiber |
| CN104233803A (en) * | 2014-09-19 | 2014-12-24 | 太仓苏纶纺织化纤有限公司 | Dip coating preparation method of modified basalt fiber/polyphenylene sulfide composite filter material |
| CN108035004A (en) * | 2017-11-20 | 2018-05-15 | 河北吉藁化纤有限责任公司 | A kind of flame retardant viscose fiber and preparation method thereof |
| CN108677351A (en) * | 2018-05-18 | 2018-10-19 | 宁波荣昌祥服饰股份有限公司 | A kind of anti-bacterial and anti-fouling shirt fabric |
| CN109137112A (en) * | 2018-08-03 | 2019-01-04 | 江南大学 | A kind of fire resistance fibre for automobile interiors and preparation method thereof |
| CN109137112B (en) * | 2018-08-03 | 2021-08-17 | 江南大学 | Flame-retardant fiber for automotive interior and preparation method thereof |
| CN111041567A (en) * | 2019-12-19 | 2020-04-21 | 阜宁澳洋科技有限责任公司 | Method for manufacturing aluminum-containing viscose fibers |
| CN112048827A (en) * | 2020-09-11 | 2020-12-08 | 秦小康 | Melt-blown short fiber spinning method and non-woven fabric filter material product prepared by same |
| CN113293449A (en) * | 2021-07-27 | 2021-08-24 | 兴晔新材料(南通)有限公司 | Preparation method of high-temperature-resistant artificial fiber |
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Effective date of registration: 20211207 Address after: 224400 Jiangsu Yancheng Funing high tech Industrial Development Zone Aoyang Avenue Saideli (Yancheng) Fiber Co., Ltd Patentee after: Saideli (Yancheng) Fiber Co.,Ltd. Address before: 224400 No. 1, Aoyang Avenue, Aoyang Industrial Park, Funing County, Yancheng City, Jiangsu Province Patentee before: FUNING AOYANG TECHNOLOGY CO.,LTD. |