CN109137112A - A kind of fire resistance fibre for automobile interiors and preparation method thereof - Google Patents
A kind of fire resistance fibre for automobile interiors and preparation method thereof Download PDFInfo
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- CN109137112A CN109137112A CN201810878161.9A CN201810878161A CN109137112A CN 109137112 A CN109137112 A CN 109137112A CN 201810878161 A CN201810878161 A CN 201810878161A CN 109137112 A CN109137112 A CN 109137112A
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- preparation
- fire
- fire resistance
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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
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of preparation method of fire resistance fibre for automobile interiors, the preparation step including fire retardant spinning glue.The preparation of the fire retardant spinning glue: first fibre content 6-10wt%, 6-9wt% containing alkali, viscosity 35-60s in fire retardant spinning glue, degree of ripeness (10%NH4Cl) 18-30ml.The preparation of the fire retardant spinning glue: in fire retardant spinning glue fire retardant effective content be 20-35wt% to first fibre, graphene 0.5-3wt%.Fiber prepared by the present invention is suitable for automobile interior decoration, good flame retardation effect.
Description
Technical field
The present invention relates to a kind of fire resistance fibres and preparation method thereof, and in particular to it is a kind of using Populus deltoides pulp as raw material, be applicable in
In automobile interior decoration, graphene modified inorganic silicon systems fire resistance fibre and preparation method thereof.
Background technique
With the development of science and technology, the fire-retardant research of automotive interior material deepens constantly, and novel flame-retardant fiber is due to it
Superior flame retardant property is also gradually applied to automobile interior decoration field.Currently, being manufactured and being hindered by additive process using Populus deltoides pulp as raw material
The method of combustion fiber is obtained fire resistance fibre after mixing fire retardant with spinning solution before spinning, and this method is in order to reach fire-retardant
The requirement of performance, the flame retardant agent content for generally requiring addition is higher, this reduces the strength of fiber to a certain extent, answers it
With being restricted.And the structure of graphene is highly stable, carbon-carbon bond is only 1.42, the company between carbon atom inside graphene
Connect very flexible, theoretical Young's modulus reaches 1.0TPa, tensile strength 130GPa.The mechanical property that we utilize graphene excellent
Can, graphene modified inorganic silicon systems fire resistance fibre is prepared under conditions of being added without other modifying agent, and it is fire-retardant to promote single silicon systems
The quality and mechanical property of fiber.
Patent CN106626656A discloses a kind of flame retardant automotive inner decoration facing compound and its application, used in it is fire-retardant
Automobile inner decoration facing is formed by phosphorous permanent fire retardant dacron through final finishing, and it is poor, not wash resistant that there are flame retardant effect persistence
The problem of.CN102286799A discloses a kind of preparation method of flame retardant viscose fiber, is added using silicon, aluminium as composite flame-retardant agent
It being added in viscose and carries out the obtained fire resistance fibre of spinning, for this method in order to reach preferable flame retardant effect, fire retardant additive amount is big,
It is larger to the strong influence of fiber.
Patent CN106367830A discloses a kind of preparation method of fire-retardant regenerated cellulose fiber, is by graphene and resistance
It is added in viscose after combustion agent mixing and carries out spinning, the fire retardant of addition is aluminium compound, magnesium compound, phosphorous flame-retardant
One or more of agent, antimonial etc., fire retardant partial size≤5000 mesh, the partial size of fire retardant added by this method compared with
Greatly, larger to the intensity effect of the spinnability of spinning and fiber.The system of flame retardant viscose fiber disclosed in patent CN103643334A
Preparation Method is to be added to zinc oxide in viscose as fire retardant to carry out spinning after blending, zinc oxide partial size≤5 μm, equally
There are problems that fire retardant partial size is larger, influences spinnability and fibre strength.
Summary of the invention
The problem to be solved in the present invention be in view of the deficiencies of the prior art, provide a kind of fire resistance fibre for automobile interiors and its
Preparation method, by the way that inorganic silicon-series five-retardant to be added in viscose and spin in the form of true solution and after graphene mixing
Silk, being made has preferable flame retardant effect and the fire resistance fibre for automobile interiors compared with high-tenacity.
Technical scheme is as follows:
A kind of preparation method of fire resistance fibre for automobile interiors, the preparation including (1) graphene emulsion, (2) fire retardant spinning glue
Preparation, (3) spinning moulding step.
Graphene is graphene oxide in the step (1);The solvent used is caustic soda;
Partial size≤3 μm of the graphene oxide;
Graphene concentration is 1-5wt% in the graphene emulsion of preparation, and the dispersant dosage of addition is graphene emulsion quality
0.5-3wt%;
The dispersing agent is one or more of dimethylformamide, calgon, polyvinyl alcohol, hydroxyethyl cellulose;
The concentration of caustic soda is 4-7wt%.
In the step (2), fire retardant is inorganic fire retardants;
The inorganic fire retardants is inorganic silicic acid salting liquid;
The inorganic silicic acid salting liquid effective component is SiO2;
In the fire retardant spinning glue, fire retardant effective content is (with SiO2Meter) it is that 20-35wt%, graphene effectively contain to first fibre
Amount is 0.5-3wt% to first fibre;
In the fire retardant spinning glue, first fibre content 6-10wt%, 6-9wt% containing alkali, viscosity (falling ball method) 35-60s, degree of ripeness
(10%NH4Cl)18-30ml。
In the step (3), coagulation bath composition is sulfuric acid 95-140g/l, zinc sulfate 20-35g/l sodium sulphate 280-
360g/l。
By adopting the above-described technical solution, the beneficial effects of the present invention are:
1, fire resistance fibre for automobile interiors is using cellulose as matrix, and wherein fire retardant effective content is (with SiO2Meter) it is 20-
35wt%, graphene are 0-3wt %, and the dry Duan of fire resistance fibre splits Qiang Du≤1.84cN/dtex, and Shi Duan splits Qiang Du≤0.96cN/
Dtex, Ci Dian≤2.4mg/100g, LOI Zhi≤30.2%, heat release rate < 16kW.
Graphene and inorganic silicon-series five-retardant can achieve the effect of cooperative flame retardant, reduce the additional amount of inorganic component, protect
Flame retardant effect is demonstrate,proved, reduces the fault of fire resistance fibre, improves fiber quality.
2, the characteristic of graphene oxide layer, high intensity, high tenacity, large specific surface area improves the mechanical property of fiber.
3, after graphene and inorganic silicon systems fire resistance fibre are compound, grey black is presented according to how much fibers of graphene content,
While promoting fiber quality, assign fiber new antibacterial, health care, colouring function.
4, after graphene and inorganic silicon systems fire resistance fibre are compound, fiber strength and anti-flammability are caused after avoiding stock-dye
The reduction of energy, has further widened application field.
Specific embodiment
Below with reference to specific embodiment, the present invention is further explained.
Embodiment 1
A kind of fire resistance fibre for automobile interiors and preparation method thereof, comprising the following steps:
(1) under conditions of being sufficiently stirred, dimethyl methyl the preparation of graphene emulsion: is added in the caustic soda for being 4% to mass concentration
Amide after being uniformly dispersed, is slowly added to graphene oxide, disperses 2h with homogenizer at 1500 rpm, uses laser particle size analyzer
Partial size D90=2.326 μm of slurry are detected, graphene emulsion is made.Wherein, the additional amount of dimethylformamide is graphene cream
The 0.5wt% of liquid quality, the additional amount of graphene oxide are the 1wt% of graphene emulsion quality.
(2) preparation of fire retardant spinning glue: preparing rayon spinning liquid with common process, by fire retardant rear dissolution process with
True solution form is added in viscose glue, is added to graphene emulsion by injecting systems before spinning using after filter, maturation, deaeration
In spinning glue.Graphene additive amount is 0.5wt%, fire retardant effective content SiO to first fibre2It is 35wt% to first fibre, it is fine that first is made
Content 6wt%, 6wt% containing alkali, viscosity (falling ball method) 40s, degree of ripeness (10%NH4Cl) the flame-retardant spinning glue of 30ml.
(3) spinning moulding: by flame-retardant spinning glue coagulation forming in coagulating bath, then, refined and drying is made
Flame retardant viscose fiber.The coagulating bath: sulfuric acid 95g/l, zinc sulfate 20g/l, sodium sulphate 280g/l.The dry of fire resistance fibre is made
Breaking strength 1.84cN/dtex, wet breaking strength 0.96cN/dtex, fault 2.4mg/100g, LOI value 30.2%, heat release
Rate is 15.72kW.
Embodiment 2
A kind of fire resistance fibre for automobile interiors and preparation method thereof, comprising the following steps:
(1) under conditions of being sufficiently stirred, 1.0wt% six preparation of graphene emulsion: is added in the caustic soda that mass concentration is 6%
Sodium metaphosphate and 0.5wt% polyvinyl alcohol, are slowly added to the graphene oxide of 3wt% after being uniformly dispersed, use homogeneous at 2000rpm
Machine disperses 3h, with partial size D90=2.235 μm of laser particle size analyzer detection slurry.
(2) preparation of fire retardant spinning glue: preparing rayon spinning liquid with common process, by fire retardant rear dissolution process with
True solution form is added in viscose glue, is added to graphene emulsion by injecting systems before spinning using after filter, maturation, deaeration
In spinning glue.Graphene additive amount is 1.5wt%, fire retardant effective content SiO to first fibre2It is 30wt% to first fibre, it is fine that first is made
Content 8wt%, 7.2wt% containing alkali, viscosity (falling ball method) 50s, degree of ripeness (10%NH4Cl) the flame-retardant spinning glue of 24ml.
(3) spinning moulding: the flame-retardant spinning glue is formed in coagulating bath, and then, refined and drying is made fire-retardant
Viscose rayon.The coagulating bath: sulfuric acid 125g/l, zinc sulfate 28g/l, sodium sulphate 320g/l.The dry disconnected of fire resistance fibre is made
Resistance to spalling 1.92cN/dtex, wet breaking strength 1.05cN/dtex, fault 1.6mg/100g, LOI value 31.6%, heat release speed
Rate is 14.06kW.
Embodiment 3
A kind of fire resistance fibre for automobile interiors and preparation method thereof, comprising the following steps:
(1) under conditions of being sufficiently stirred, 0.5wt% six preparation of graphene emulsion: is added in the caustic soda that mass concentration is 7%
Sodium metaphosphate and 1.5wt% hydroxyethyl cellulose, are slowly added to the graphene oxide of 5wt% after being uniformly dispersed, use at 2500rpm
Homogenizer disperses 3.5h, with partial size D90=1.968 μm of laser particle size analyzer detection slurry.
(2) preparation of fire retardant spinning glue: preparing rayon spinning liquid with common process, and fire retardant and graphene emulsion are used
It after 20min is mixed in homogenizer, is added in viscose glue in rear dissolution process, is hindered using mixing is made after filter, maturation, deaeration
Fire spinning glue.Graphene additive amount is 3wt%, fire retardant effective content SiO to first fibre2It is 20wt% to first fibre, first fibre is made and contains
Measure the flame-retardant spinning glue of 9.4wt%, 8.6wt% containing alkali, viscosity (falling ball method) 58s, degree of ripeness (10%NH4Cl) 18ml.
(3) spinning moulding: the flame-retardant spinning glue is formed in coagulating bath, and then, refined and drying is made fire-retardant
Viscose rayon.The coagulating bath: sulfuric acid 140g/l, zinc sulfate 35g/l, sodium sulphate 360g/l.The dry disconnected of fire resistance fibre is made
Resistance to spalling 2.12cN/dtex, wet breaking strength 1.22cN/dtex, fault 0.8mg/100g, LOI value 33.2%, heat release speed
Rate is 12.18kW.
Comparative example
It is same as Example 1, only change: the inorganic silicate fire retardant of identical mass fraction is added, is added without graphene.
The dry breaking strength 1.52cN/dtex, wet breaking strength 0.75cN/dtex, fault 4.5mg/ of fire resistance fibre is made
100g, LOI value 28.6%, heat release rate 18.64kW.
In addition to specified otherwise, percentage of the present invention is mass percent, and the ratio is mass ratio.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of preparation method of fire resistance fibre for automobile interiors, it is characterised in that: the preparation step including fire retardant spinning glue.
2. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 1, it is characterised in that: described fire-retardant
The preparation of agent spinning glue: first fibre content 6-10wt%, 6-9wt% containing alkali, viscosity 35-60s, degree of ripeness in fire retardant spinning glue
(10%NH4Cl)18-30ml。
3. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 1, it is characterised in that: described fire-retardant
The preparation of agent spinning glue: in fire retardant spinning glue fire retardant effective content be 20-35wt% to first fibre, graphene 0.5-3wt%.
4. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 1, it is characterised in that: described fire-retardant
Agent is inorganic fire retardants, and the inorganic fire retardants is inorganic silicic acid salting liquid.
5. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 1, it is characterised in that: the system
Preparation Method further includes the preparation step of graphene emulsion;
The preparation of the graphene emulsion: the graphene is graphene oxide;The solvent used is caustic soda.
6. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 5, it is characterised in that: the stone
The preparation of black alkene lotion: partial size≤3 μm of graphene oxide;Graphene concentration is 1-5wt% in the graphene emulsion of preparation, is added
The dispersant dosage entered is the 0.5-3wt% of graphene emulsion quality.
7. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 6, it is characterised in that: the dispersion
Agent is one or more of dimethylformamide, calgon, polyvinyl alcohol, hydroxyethyl cellulose.
8. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 5, it is characterised in that: the caustic soda
Concentration is 4-7wt%.
9. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 1, it is characterised in that: the system
Preparation Method further includes spinning moulding step;
The spinning moulding: the coagulation bath composition used is sulfuric acid 95-140g/l, zinc sulfate 20-35g/l sodium sulphate 280-
360g/l。
10. a kind of preparation method of fire resistance fibre for automobile interiors according to claim 1, it is characterised in that: preparation
The dry Duan of fire resistance fibre for automobile interiors splits Qiang Du≤1.84cN/dtex, and Shi Duan splits Qiang Du≤0.96cN/dtex, and Ci Dian≤
2.4mg/100g, LOI Zhi≤30.2%, heat release rate < 16kW.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102286799A (en) * | 2011-08-22 | 2011-12-21 | 阜宁澳洋科技有限责任公司 | Fire-retardant viscose fiber and preparation method thereof |
CN105220255A (en) * | 2015-10-20 | 2016-01-06 | 恒天海龙股份有限公司 | Fire-retardant regenerated celulose fibre of Bepaint inorganic and preparation method thereof |
CN106367830A (en) * | 2016-08-30 | 2017-02-01 | 江苏金太阳纺织科技股份有限公司 | Preparation method of flame-retardant regenerated cellulose fibers |
CN106626656A (en) * | 2017-01-09 | 2017-05-10 | 杭州湘隽纺织阻燃科技有限公司 | Flame-retardant automobile trim fabric composite and application thereof |
-
2018
- 2018-08-03 CN CN201810878161.9A patent/CN109137112B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102286799A (en) * | 2011-08-22 | 2011-12-21 | 阜宁澳洋科技有限责任公司 | Fire-retardant viscose fiber and preparation method thereof |
CN105220255A (en) * | 2015-10-20 | 2016-01-06 | 恒天海龙股份有限公司 | Fire-retardant regenerated celulose fibre of Bepaint inorganic and preparation method thereof |
CN106367830A (en) * | 2016-08-30 | 2017-02-01 | 江苏金太阳纺织科技股份有限公司 | Preparation method of flame-retardant regenerated cellulose fibers |
CN106626656A (en) * | 2017-01-09 | 2017-05-10 | 杭州湘隽纺织阻燃科技有限公司 | Flame-retardant automobile trim fabric composite and application thereof |
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