CN105780175B - A kind of flame retardant viscose fiber and preparation method thereof - Google Patents
A kind of flame retardant viscose fiber and preparation method thereof Download PDFInfo
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- CN105780175B CN105780175B CN201610343351.1A CN201610343351A CN105780175B CN 105780175 B CN105780175 B CN 105780175B CN 201610343351 A CN201610343351 A CN 201610343351A CN 105780175 B CN105780175 B CN 105780175B
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- melamine
- flame retardant
- viscose
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
Abstract
The present invention provides a kind of preparation method of flame retardant viscose fiber, the preparation method includes following technique: synthesizing a kind of modified melamine-formaldehyde resin as flame retardant solution, flame retardant solution is quickly blended with viscose solution again, flame retardant viscose fiber is made using conventional spinning.The preparation method technological operation of flame retardant viscose fiber provided by the invention is simple, the flame retardant viscose fiber made from this method has preferable flame-proof heat-resistant effect, limit oxygen index (LOI value) can be improved to 29%, compared with the limit oxygen index (LOI value) 19% of common viscose fiber compared to improving 6-10%.The addition of modified cyanurotriamide resin does not influence the spinning moulding of fiber, and spinning properties are preferable.
Description
Technical field
The invention belongs to cellulose viscose fiber technical field more particularly to a kind of flame retardant viscose fiber and its preparation sides
Method.
Background technique
Viscose rayon has a series of valuable physical mechanical properties and meets the property of hygienic requirements.As a kind of regeneration
Cellulose fibre, its biggest characteristic is that certain properties with cotton fiber are extremely similar, it is comfortable and easy to wear, it is particluarly suitable for hot climate
Area dress, and its fiber number and length can be adjusted according to the requirement of purposes, therefore welcomed by the people.But it is general
It directly burns after logical viscose rayon contact flame, withdraws still sustained combustion after fire source, burning velocity is fast and without ash.Inflammability
Disadvantage as viscose rayon maximum.
Research for viscose rayon anti-flammability, many patents all relate to, such as Chinese patent CN102505169A public
A kind of flame retardant viscose fiber and preparation method thereof has been opened, has been added according to a certain percentage by sodium metasilicate, pyrophosphate solution
It is uniformly mixed into the cellulose viscose solution after yellow, flame-retardant spinning viscose solution is prepared, by using conventional spinning
Silk technology, is finally made flame retardant viscose fiber product, but the method for modifying belongs to simple physical blending process, this method can make
Fire retardant mixes unevenness with viscose solution, influences the flame retardant property of fiber, and the fire retardant is easy sedimentation and reunites, and then influences
The spinnability of viscose rayon；Chinese patent CN103643334A, which is disclosed, a kind of as fire retardant is added to viscose glue using zinc oxide
Method in solution to prepare flame retardant viscose fiber, but zinc oxide is present in viscose rayon with graininess, due to wet process
The aperture of spinning nozzle is smaller, and Zinc oxide particles, which are easy blocking spinneret, influences its spinnability, brings one to continuous production
Fixed difficulty, and flame retardant effect is not fine；Chinese patent CN104178836A disclose a kind of fire retardant viscose short filament and
Preparation method, the fire retardant viscose short filament are to add before spinning using organophosphorus ester as the phosphorus flame retardant next life of effective component
It producing, phosphorus flame retardant therein is the new penta diester fire retardant suspension of phosphordithiic acid generated by series reaction, by
It is to take water as a solvent in viscose, the fire retardant and viscose solution are simple physical blending, are asked there are number of dropouts is biggish
Topic.
Summary of the invention
It is insufficient to solve the prior art, the purpose of the present invention is to provide a kind of flame retardant viscose fiber and preparation method thereof,
Compared with common viscose fiber, flame-retardance and thermal endurance improves the flame retardant viscose fiber.
The technical solution that the present invention solves the technical problem is to design a kind of preparation method of flame retardant viscose fiber, should
Preparation method includes following technique: preparing a kind of flame retardant viscose fiber, the main component of the fiber includes the fiber of 50-90%
Element, the modified melamine-formaldehyde resin of 10-50%；The modified melamine-formaldehyde resin, including chemical modification and altogether
Mixed modification two parts；The chemical modification, modifying agent be one of urea or diethyl ethylphosphate, modifying agent with
The molar ratio of melamine is 0.1-0.5: 1；The blending and modifying, modifying agent are two (dioctyl phosphito of tetra isopropyl
Acyloxy) titanate esters, 3- aminopropyl triethoxysilane or three kinds of propyl trimethoxy silicane of γ-(2,3- glycidoxy) increasings
One of tough modifying agent, the additive amount of modifying agent are the 0.2-5% of melamine resin mass percent；Described changes
Property melamine resin in, select that sodium hydroxide solution, sodium carbonate liquor, oxalic acid, hydrochloric acid is as pH adjusting agent.
The technical solution that the present invention solves the technical problem is to design a kind of flame retardant viscose fiber, it is characterised in that is adopted
It is prepared with above-mentioned preparation method, limit oxygen index (LOI value) can be improved to 29%, compared with the limit oxygen index of common viscose fiber
(LOI value) 19% improves 6-10%, while meeting national and related environmental protection standard in the world requirement.
Compared with prior art, design scheme of the present invention is to utilize shape between modified melamine-formaldehyde resin and cellulose
The characteristics of at hydrogen bond and chemical bond, the compatibility of resin and viscose rayon is improved, while improving resin containing in viscose rayon
Amount, to reach good flame retardant effect.Its simple process, easy to operate, manufacturing cost relative moderate, modified melamine-formaldehyde
The addition of resin does not influence the spinning moulding of fiber, and flame retardant viscose fiber good physical performance obtained has preferable fire-retardant, resistance to
Heat, suppression cigarette and other effects.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
A kind of preparation method of flame retardant viscose fiber (abbreviation preparation method) of the present invention, it is characterised in that operating procedure is such as
Under:
(1) melamine resin solution is configured.In molar ratio it is 1: 1.5-4.5, weighs a certain amount of melamine
With paraformaldehyde in there-necked flask, suitable distilled water is added, is warming up to 30-50 DEG C under agitation, after solution clarification,
PH value is adjusted, control is warming up to 70-95 DEG C in pH=7-9, reacts 20-60min；
(2) to melamine resin solution modification.It is cooled to 40-60 DEG C, urea or diethyl ethylphosphate is added,
10-30min is reacted, pH value is adjusted, control is added plasticized modifier, is warming up to 70-95 DEG C, controls in reaction process in pH=5-9
PH processed reacts 0.5-2.5 hours between 5-9, obtains modified melamine-formaldehyde resin；
(3) spinning moulding of flame retardant viscose fiber.Suitable viscose solution is weighed, modified melamine-formaldehyde resin is added
It is added in viscose solution, the mass ratio of cellulose is 50-10: 50-90 in modified melamine-formaldehyde resin and viscose solution, warp
The techniques such as quick stirring, vacuum defoamation, spinning moulding, drawing-off, washing, desulfurization, drying process are crossed, anti-flaming viscose is finally prepared into
Fiber.
Preferred tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters of the plasticized modifier, three ethoxy of 3- aminopropyl
One of base silane or γ-(2,3- glycidoxy) propyl trimethoxy silicane.
Flame retardant property test: fiber samples are weaved into the column sample of 10mm*5mm*100mm, are carried out in oxygen index instrument
Limit oxygen index measurement.
Through testing, preparation method of the present invention is even more ideal using the effect of following process parameters range:
(1) melamine resin solution is configured.In molar ratio it is 1: 1.5-4.5, weighs a certain amount of melamine
With paraformaldehyde in there-necked flask, suitable distilled water is added, is warming up to 30-50 DEG C under agitation, after solution clarification,
PH value is adjusted, control is warming up to 70-95 DEG C in pH=7-9, reacts 30-60min；
(2) to melamine resin solution modification.Be cooled to 40-60 DEG C, by urea or diethyl ethylphosphate with
Melamine molar ratio is 0.1-0.4: 1 addition one of urea or diethyl ethylphosphate, reacts 20-30min, adjusts pH
The plasticized modifier of resin quality percentage 1-5% is added in pH=5-9 in value, control, is warming up to 70-95 DEG C, in reaction process
PH is controlled between 5-9, reacts 0.5-2.0 hours, obtains modified melamine-formaldehyde resin；
(3) spinning moulding of flame retardant viscose fiber.Suitable viscose solution is weighed, modified melamine-formaldehyde resin is added
It is added in viscose solution, the mass ratio of cellulose is 50-10: 50-90 in modified melamine-formaldehyde resin and viscose solution, warp
The techniques such as quick stirring, vacuum defoamation, spinning moulding, drawing-off, washing, desulfurization, drying process are crossed, anti-flaming viscose is finally prepared into
Fiber.
Flame retardant viscose fiber of the present invention, which is characterized in that and general using the flame retardant viscose fiber of above-mentioned preparation method preparation
Logical viscose rayon is compared, and limit oxygen index improves 6-10%.
Embodiment 1:
In molar ratio it is 1: 1.5, weighs melamine 201.79g, paraformaldehyde 72.0g in there-necked flask, distillation is added
Water 410.69g is warming up to 30 DEG C under agitation, after solution clarification, adjusts pH value with sodium hydroxide solution, controls in pH
=9,70 DEG C are warming up to, 60min is reacted；40 DEG C are cooled to, is added by diethyl ethylphosphate and melamine molar ratio 0.3: 1
79.76g diethyl ethylphosphate reacts 30min, with careless acid for adjusting pH value, controls in pH=5, the tetra isopropyl of 0.55g is added
Two (dioctyl phosphito acyloxy) titanate esters plasticized modifiers are warming up to 70 DEG C, react 0.5 hour, control in reaction process
PH=5；1000g viscose solution is weighed, wherein content of cellulose is 8% in viscose solution, by modified melamine-formaldehyde resin
Mass ratio with cellulose in viscose solution is 35: 65, and 43.08g modified melamine-formaldehyde resin is added to viscose solution
In, by quickly stirring, vacuum defoamation, spinning moulding, drawing-off, washing, desulfurization, the conventional spinning processes such as drying process, finally
It is prepared into flame retardant viscose fiber.Through detecting, the limit oxygen index (LOI value) of fiber is 28%.
Embodiment 2:
In molar ratio it is 1: 3.0, weighs melamine 201.79g, paraformaldehyde 144g in there-necked flask, distilled water is added
518.69g is warming up to 50 DEG C under agitation, after solution clarification, adjusts pH value with sodium hydroxide solution, controls in pH=
7,95 DEG C are warming up to, 20min is reacted；60 DEG C are cooled to, is added by diethyl ethylphosphate and melamine molar ratio 0.4: 1
106.34g diethyl ethylphosphate reacts 10min, with careless acid for adjusting pH value, controls in pH=9, four isopropyls of 6.92g are added
Base two (dioctyl phosphito acyloxy) titanate esters plasticized modifier is warming up to 95 DEG C, reacts 2.5 hours, controls in reaction process
PH=9 processed；Claim 1000g viscose solution, wherein content of cellulose is 8% in viscose solution, by modified melamine-formaldehyde resin
Mass ratio with cellulose in viscose solution is 40: 60, and 53.33g modified melamine-formaldehyde resin is added to viscose solution
In, by quickly stirring, vacuum defoamation, spinning moulding, drawing-off, washing, desulfurization, the conventional spinning processes such as drying process, finally
It is prepared into flame retardant viscose fiber.Through detecting, the limit oxygen index (LOI value) of fiber is 29%.
Embodiment 3:
In molar ratio it is 1: 4.5, weighs melamine 201.79g, paraformaldehyde 216g in there-necked flask, distilled water is added
626.69g is warming up to 65 DEG C under agitation, after solution clarification, adjusts pH value with sodium hydroxide solution, controls in pH=
8,80 DEG C are warming up to, 30min is reacted；40 DEG C are cooled to, 48.05g urea is added by urea and melamine molar ratio 0.5: 1,
10min is reacted, with salt acid for adjusting pH value, controls in pH=6, the 3- aminopropyl triethoxysilane toughening modifying of 12.53g is added
Agent is warming up to 80 DEG C, reacts 1.5 hours, pH=7 is controlled in reaction process；1000g viscose solution is weighed, wherein viscose solution
Middle content of cellulose is 8%, and the mass ratio by cellulose in modified melamine-formaldehyde resin and viscose solution is 35: 65, will
43.08g modified melamine-formaldehyde resin is added in viscose solution, by quickly stirring, vacuum defoamation, spinning moulding, leads
It stretches, wash, desulfurization, the conventional spinning processes such as drying process, being finally prepared into flame retardant viscose fiber.Through detecting, the limit of fiber
Oxygen index (OI) (LOI value) is 28%.
Embodiment 4:
In molar ratio it is 1: 3.5, weighs 201.79g melamine, paraformaldehyde 168g in there-necked flask, distilled water is added
554.69g is warming up to 65 DEG C under stirring conditions, after solution clarification, adjusts pH value with sodium carbonate liquor, controls in pH=
7,85 DEG C are warming up to, 40min is reacted；45 DEG C are cooled to, is added by diethyl ethylphosphate and melamine molar ratio 0.3: 1
79.76g diethyl ethylphosphate reacts 15min, with careless acid for adjusting pH value, controls in pH=5, the 3- ammonia third of 11.09g is added
Ethyl triethoxy silicane alkane plasticized modifier is warming up to 85 DEG C, reacts 0.5 hour, pH=6 is controlled in reaction process；Weigh 1000g
Viscose solution, wherein content of cellulose is 8% in viscose solution, by fiber in modified melamine-formaldehyde resin and viscose solution
The mass ratio of element is 30: 70, and 34.29g modified melamine-formaldehyde resin is added in viscose solution, by quickly stirring,
The conventional spinning processes such as vacuum defoamation, spinning moulding, drawing-off, washing, desulfurization, drying process are finally prepared into anti-flaming viscose fibre
Dimension.Through detecting, the limit oxygen index (LOI value) of fiber is 28%.
Embodiment 5:
In molar ratio it is 1: 2.0, weighs 201.79g melamine, paraformaldehyde 96.0g in there-necked flask, distillation is added
Water 446.69g is warming up to 60 DEG C under agitation, after solution clarification, adjusts pH value with sodium carbonate liquor, controls in pH=
7,85 DEG C are warming up to, 45min is reacted；40 DEG C are cooled to, 9.61g urea is added by urea and melamine molar ratio 0.1: 1, instead
15min is answered, with salt acid for adjusting pH value, controls in pH=6, the 3- aminopropyl triethoxysilane plasticized modifier of 8.93g is added,
85 DEG C are warming up to, reacts 1.2 hours, pH=7 is controlled in reaction process；1000g viscose solution is weighed, it is wherein fine in viscose solution
Tieing up cellulose content is 8%, and the mass ratio by cellulose in modified melamine-formaldehyde resin and viscose solution is 10: 90, by 8.89g
Modified melamine-formaldehyde resin is added in viscose solution, by quickly stirring, vacuum defoamation, spinning moulding, drawing-off, water
It washes, desulfurization, the conventional spinning processes such as drying process, is finally prepared into flame retardant viscose fiber.Through detecting, the limit oxygen index of fiber
(LOI value) is 25%.
Embodiment 6:
In molar ratio it is 1: 2.5, weighs 201.79g melamine, paraformaldehyde 120g in there-necked flask, distilled water is added
482.69g is warming up to 60 DEG C under agitation, after solution clarification, adjusts pH value with sodium hydroxide solution, controls in pH=
8,80 DEG C are warming up to, 50min is reacted；40 DEG C are cooled to, 19.22g urea is added by urea and melamine molar ratio 0.2: 1,
20min is reacted, with salt acid for adjusting pH value, controls in pH=7, γ-(2,3- glycidoxy) propyl front three of 16.09g is added
Oxysilane plasticized modifier is warming up to 85 DEG C, reacts 0.5 hour, pH=6 is controlled in reaction process；It is molten to weigh 1000g viscose glue
Liquid, wherein content of cellulose is 8% in viscose solution, by the matter of cellulose in modified melamine-formaldehyde resin and viscose solution
Amount than be 50: 50,80g modified melamine-formaldehyde resin is added in viscose solution, by quickly stirring, vacuum defoamation,
The conventional spinning processes such as spinning moulding, drawing-off, washing, desulfurization, drying process, are finally prepared into flame retardant viscose fiber.Through detecting,
The limit oxygen index (LOI value) of fiber is 29%.
Claims (3)
1. a kind of flame retardant viscose fiber, it is characterised in that: the main component of the fiber includes the cellulose of 50-90%, 10-50%
Modified melamine-formaldehyde resin, in modified melamine-formaldehyde resin, the molar ratio of melamine and paraformaldehyde is 1:
1.5-4.5, and using water as solvent, the content of water is the 60% of melamine resin, the modified cyanurotriamide first
Urea formaldehyde, including chemical modification and blending and modifying two parts, the chemical modification of melamine resin, modifying agent are ethyl
Diethyl phosphonate is a kind of, and the molar ratio with melamine is 0.1-0.5: 1, and the blending and modifying of melamine resin changes
Property reagent be tetra isopropyl two (dioctyl phosphito acyloxy) titanate esters, 3- aminopropyl triethoxysilane or γ-(2,3- rings
One of oxygen propoxyl group) three kinds of plasticized modifiers of propyl trimethoxy silicane, additive amount is melamine resin matter
Measure the 0.2-5%, limit oxygen index (LOI value) 25-29% of the flame retardant viscose fiber of percentage.
2. flame retardant viscose fiber according to claim 1, it is characterised in that: the modified melamine-formaldehyde resin
Preparation step is as follows:
(1) in molar ratio it is 1: 1.5-4.5, weighs a certain amount of melamine and paraformaldehyde in there-necked flask, is added appropriate
Distilled water, be warming up to 30-50 DEG C under agitation, to solution clarify；
(2) pH value is adjusted, control is warming up to 70-95 DEG C in pH=7-9, reacts 20-60min；
(3) it is cooled to 40-60 DEG C, diethyl ethylphosphate is added, reacts 10-30min；
(4) pH value is adjusted, plasticized modifier is added between 5-9 in control pH in reaction process, is warming up to 70-95 DEG C, is blended anti-
It answers 0.5-2.5 hours, obtains modified melamine-formaldehyde resin.
3. a kind of preparation method of flame retardant viscose fiber according to claim 2, it is characterised in that: by modified cyanurotriamide
Formaldehyde resin is added in viscose solution, and the mass ratio of cellulose is 50- in modified melamine-formaldehyde resin and viscose solution
10: 50-90, by quickly stirring, vacuum defoamation, spinning moulding, drawing-off, washing, desulfurization, dry treatment process, it is prepared into resistance
Fire viscose rayon.
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Families Citing this family (5)
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| CN106567195A (en) * | 2016-11-01 | 2017-04-19 | 安徽依采妮纤维材料科技有限公司 | Anti-flaming and wear-resisting non-woven fabric material |
| CN107268331A (en) * | 2017-07-25 | 2017-10-20 | 攀枝花学院 | Impregnate paper glue modifying agent and preparation method thereof |
| CN109183409B (en) * | 2018-08-16 | 2020-10-13 | 重庆消防安全技术研究服务有限责任公司 | Method for preparing flame-retardant viscose fiber from melamine grafted oxidized viscose fiber and flame-retardant viscose fiber |
| CN111041610B (en) * | 2020-01-07 | 2022-09-09 | 郑州中科新兴产业技术研究院 | Melamine/cellulose flame-retardant material and preparation method thereof |
| CN111691197B (en) * | 2020-06-24 | 2021-06-25 | 常州市佳胜无纺布有限公司 | Washable flame-retardant non-woven fabric and preparation method thereof |
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| CN1344821A (en) * | 2001-06-26 | 2002-04-17 | 天津工业大学 | Fire-retardant fiber and its making process |
| CN1668801A (en) * | 2002-06-20 | 2005-09-14 | 乔治亚大学研究基金会公司 | A durable flame retardant finish for cellulosic materials |
| CN102675575A (en) * | 2012-04-28 | 2012-09-19 | 南通紫鑫实业有限公司 | Preparation method of melamine formaldehyde resin for foam |
| CN104233510A (en) * | 2014-10-16 | 2014-12-24 | 恒天海龙股份有限公司 | Amino resin reinforced cellulosic fiber and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103146075A (en) * | 2013-04-10 | 2013-06-12 | 苏州旭光聚合物有限公司 | Glass fiber flame resistant polypropylene and production method thereof |
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| CN1344821A (en) * | 2001-06-26 | 2002-04-17 | 天津工业大学 | Fire-retardant fiber and its making process |
| CN1668801A (en) * | 2002-06-20 | 2005-09-14 | 乔治亚大学研究基金会公司 | A durable flame retardant finish for cellulosic materials |
| CN102675575A (en) * | 2012-04-28 | 2012-09-19 | 南通紫鑫实业有限公司 | Preparation method of melamine formaldehyde resin for foam |
| CN104233510A (en) * | 2014-10-16 | 2014-12-24 | 恒天海龙股份有限公司 | Amino resin reinforced cellulosic fiber and preparation method thereof |
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