CN108342788A - A kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof - Google Patents
A kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof Download PDFInfo
- Publication number
- CN108342788A CN108342788A CN201710054187.7A CN201710054187A CN108342788A CN 108342788 A CN108342788 A CN 108342788A CN 201710054187 A CN201710054187 A CN 201710054187A CN 108342788 A CN108342788 A CN 108342788A
- Authority
- CN
- China
- Prior art keywords
- composite fiber
- polylactic
- pla composite
- combustion inhibitor
- organic boron
- 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.)
- Pending
Links
Classifications
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
- Multicomponent Fibers (AREA)
Abstract
The invention discloses a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof, by organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin, these three components form the PLA Composite Fiber.It is described that preparation method includes the following steps：S1) composite polylactic acid master batch is produced using a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin；S2) PLA Composite Fiber is produced using the polylactic resin of a certain amount of composite polylactic acid master batch and equivalent.The PLA Composite Fiber is difficult to light in butane gas flame under the conditions of normal air, light once in a while turning off stove also can self-extinguishment do not cause lower section flocking phenomenon on fire without apparent molten drop phenomenon yet.In addition, in cone calorimetry test, the smoke density that the more typical phosphor-containing flame-proof acid fiber by polylactic of the PLA Composite Fiber generates in burning is significantly reduced more than 80%.
Description
Technical field
The present invention relates to functional form green fiber preparation fields, enhanced poly- more specifically to a kind of flame-retardant smoke inhibition
Lactic acid composite fibre and preparation method thereof.
Background technology
With the application of biodegradable green polylactic resin, the inflammable safety problem of Related product is badly in need of
It solves.
For this purpose, the Chinese patent of Publication No. CN104031364A discloses a kind of enhancing flame-retardant polylactic acid material, it is described
Enhancing flame-retardant polylactic acid material mixed by polylactic acid, modified bluish dogbane, boron bakelite resin, macromolecule polycondenseng phosphate,
The polylactic acid, modified bluish dogbane, boron bakelite resin, macromolecule polycondenseng phosphate mass ratio be 70：10：(2.5~10)：
(10~17.5), the modified bluish dogbane are that bluish dogbane is carried out alkali process, are dried after being washed to neutrality；Bluish dogbane after drying is placed in
Magnetic agitation in the ethanol water of vinyltrimethoxysilane, filters, and alcohol is washed, obtained after drying.It is a large amount of due to having inserted
Natural bluish dogbane, cause the enhancing flame-retardant polylactic acid material be not suitable for spinning processing, in addition boron bakelite resin is thermosetting property tree
Fat just need to conveniently insert after crushing and processing, and boron oxygen carbon key facile hydrolysis therein and lead to the loss of boron.
In addition, the Chinese patent of Publication No. CN103122498A discloses a kind of preparation of halogen-free flame-retardant polylactic acid fiber
Method, including：(1) polylactic acid slice and fire retardant are mixed, under the conditions of 180~220 DEG C, melt blending, cooling granulation obtains
To flame-proof polylactic acid master batch；Wherein retardant load level is the 20~50% of polylactic acid slice quality；(2) by polylactic acid slice and
Synergist mixes, and under the conditions of 190~220 DEG C, melt blending, cooling granulation obtains collaboration polylactic acid master batch；Wherein synergist
Addition be polylactic acid slice quality 5~25%；(3) polylactic acid slice, flame-proof polylactic acid master batch, collaboration polylactic acid is female
Grain, dispersant, mixing carry out spinning, obtain as-spun fibre, then hinder as-spun fibre to get Halogen using drawing-off post-processing
Fire acid fiber by polylactic, wherein flame retardant agent content is the 2~10% of gross mass, and collaboration agent content is the 0.5%~3% of gross mass,
Dispersant is the 0.1~2% of gross mass.Fire retardant is melamine, melamine cyanurate, three in the step (1)
One or more of poly cyanamid Quadrafos, triphenyl phosphate, ammonium polyphosphate.
It should be pointed out that phosphonium flame retardant, which meets fire, easily generates a large amount of poison gas, in addition, phosphonium flame retardant is certainly
The accumulation on right boundary can directly result in the eutrophication of water body, promote algae hyperplasia and bring extinction to many aquatic organisms, beat
Break the balance sustainable development of ecology.Likewise, largely using the polylactic resin of phosphonium flame retardant and fiber it is inevitable there is also with
Upper problem.
For this reason, it is necessary to design a kind of new flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof, with gram
Take the above problem.
Invention content
The technical problem to be solved in the present invention is, for existing PLA Composite Fiber due to largely using phosphor-containing flame-proof
Agent and cause meet fire easily lead to the problem of a large amount of poison gas, a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre is provided
And preparation method thereof, the PLA Composite Fiber is difficult to light in butane gas flame under the conditions of normal air, once in a while point
Fire turning off stove also can self-extinguishment do not cause lower section flocking phenomenon on fire without apparent molten drop phenomenon yet.In addition, in taper amount
In the test of hot instrument, smoke density that the more typical phosphor-containing flame-proof acid fiber by polylactic of the PLA Composite Fiber generates in burning
It significantly reduces more than 80%.
Technical solution is used by the present invention solves the problems, such as it：
On the one hand, the present invention provides a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre, the PLA Composite Fiber
By organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin, these three components form.
In PLA Composite Fiber provided by the invention, in the PLA Composite Fiber, the organic boron nitrogen is fire-retardant
The mass percentage of agent is less than or equal to 7.5%.
In PLA Composite Fiber provided by the invention, the molecular weight of the organic boron nitrogen combustion inhibitor is 160-
100000。
It is former comprising nitrogen in the molecular structure of the organic boron nitrogen combustion inhibitor in PLA Composite Fiber provided by the invention
Son, boron atom and phenyl ring, wherein boron atom is directly connected by covalent bond with phenyl ring, and the quantity of boron atom is less than nitrogen-atoms
Quantity.
In PLA Composite Fiber provided by the invention, the fire retarding synergist includes natural polymer and phosphorous chemical combination
Object.
In PLA Composite Fiber provided by the invention, the natural polymer is selected from cellulose, lignin and starch
In any one.
In PLA Composite Fiber provided by the invention, the phosphorus-containing compound is selected from boron phosphate, ammonium polyphosphate and plant
Any one in sour ammonium
Correspondingly, the present invention also provides a kind of preparation method of above-mentioned PLA Composite Fiber, include the following steps：
S1) composite polylactic acid mother is produced using a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin
Grain；
S2) polylactic acid is produced using the polylactic resin of a certain amount of composite polylactic acid master batch and equivalent
Composite fibre.
In preparation method provided by the invention, the step S1) include the following steps：
S1a a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin) is taken to be placed in certain temperature
Dry a period of time in baking oven；
S1b) organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin are weighed respectively by certain mass percent,
Wherein, the mass percent of the organic boron nitrogen combustion inhibitor and fire retarding synergist and be less than or equal to 30%, the organic boron
The mass percent of nitrogen combustion inhibitor is less than or equal to 15%；
S1c) the organic boron nitrogen combustion inhibitor, fire retarding synergist and the polylactic resin that weigh are placed in high speed mixer
Blended under agitation obtains blend composition；
S1d) blend composition is injected in Multi-stage heating double screw extruder and carries out melt blending, extrusion, granulation, do
It is dry, the composite polylactic acid master batch is made.
In preparation method provided by the invention, the step S1a) in the grain size of the fire retarding synergist be less than or wait
In 1 micron.
Compared with prior art, implement PLA Composite Fiber provided by the invention and preparation method thereof, have has as follows
Beneficial effect：
1, the PLA Composite Fiber is by these three components of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin
Composition.The PLA Composite Fiber not only has efficient flame retardant property but also can effectively inhibit the generation of smog as a result,.
2, the fire retarding synergist includes natural polymer and phosphorus-containing compound, thus, it is possible to be effectively prevented from described poly-
Molten drop phenomenon occurs for lactic acid composite fibre.
3, good mechanical strength is had according to PLA Composite Fiber made from preparation method provided by the invention, be suitble to
Textile process and the requirement used.Moreover, remaining to keep every superperformance after the washing of multiple standard.
Specific implementation mode
For a clearer understanding of the technical characteristics, objects and effects of the present invention, what now the present invention will be described in detail
Specific implementation mode.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Based on the embodiments of the present invention, what those of ordinary skill in the art were obtained without creative efforts is all
Other embodiment shall fall within the protection scope of the present invention.
First, in order to preferably embody the present embodiment compared with the existing technology the advantages of, we are previously prepared one
Plant a kind of PLA Composite Fiber containing melamine polyphosphate having disclosed in the prior art sample as a comparison.
The preparation of comparative sample
A certain amount of melamine polyphosphate, microcrystalline cellulose and polylactic resin is taken to be done in 120 ± 5 DEG C of baking oven
Dry 24 hours.Weigh the polylactic resin and 2.0kg drying melamine Quadrafos of 7.0kg dryings, 1.0kg microcrystalline celluloses
It is placed in blended under agitation in high speed mixer, is then injected in Multi-stage heating double screw extruder and is carried out melt blending, squeeze out, make
Grain, drying, extrusion temperature are 180 DEG C.In gained composite polylactic acid pellet, mass percent shared by melamine polyphosphate is about
20%.Pass through melt spinning machine spinning, drawing-off and volume by 50/50 mixing with polylactic resin with gained composite polylactic acid masterbatch
Around etc. techniques continuous composite flame retardant fiber is made.Wherein, hot gas spring temperature is 80 DEG C.
The properties of comparative sample
Weavability：
The line density of gained comparative sample is 4.5dtex, and the surface of fracture strength 2.6cN/dtex, gained comparative sample are smooth,
With good weavability.
Anti-flammability：
It is tested according to GB/T5454-1997 (textile combustion performance test oxygen index method), the LOI values of the comparative sample are
33.5；
Smoke-suppressing
It is tested according to GB/T16172-2007 (construction material heat release rate test method) using cone calorimetry, this
The smoke density (SEA) of comparative sample is denoted as 100%.
Embodiment one
The present embodiment provides a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibres and preparation method thereof.
PLA Composite Fiber
The PLA Composite Fiber is by these three component groups of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin
At.
Specifically, the characteristics of organic boron nitrogen combustion inhibitor, is：Molecular weight is 160-100000, is wrapped in molecular structure
Nitrogen atom, boron atom and phenyl ring, wherein boron atom is directly connected by covalent bond with phenyl ring, and the quantity of boron atom is less than
The quantity of nitrogen-atoms.The mass percentage of the organic boron nitrogen combustion inhibitor can be less than or equal to 7.5% arbitrary value.Institute
It includes natural polymer and phosphorus-containing compound to state fire retarding synergist, wherein the natural polymer be selected from cellulose, lignin and
Any one in starch, any one of the phosphorus-containing compound in boron phosphate, ammonium polyphosphate and phytic acid ammonium.
In the present embodiment, the organic boron nitrogen combustion inhibitor is contraposition amino nitrile phenyl boric acid (molecular weight 161, boron content
6.2%), the fire retarding synergist is the mixture of microcrystalline cellulose and boron phosphate.In other words, provided in this embodiment described poly-
Lactic acid composite fibre is made of contraposition amino nitrile phenyl boric acid, microcrystalline cellulose, boron phosphate and polylactic resin, wherein described right
The mass percent of bit amino nitrile phenyl boric acid is about 7.5%.
The preparation of PLA Composite Fiber
S1) composite polylactic acid mother is produced using a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin
Grain.Wherein, the grain size of the fire retarding synergist is less than or equal to 1 micron.
In the present embodiment, it is specifically divided into following steps：
S1a a certain amount of contraposition amino nitrile phenyl boric acid (molecular weight 161, boron content 6.2%), microcrystalline cellulose, phosphoric acid) are taken
Boron and polylactic resin are 24 hours dry in 120 ± 5 DEG C of baking oven.
S1b the polylactic resin and 1.5kg drying amino nitrile phenyl boric acids of 7.0kg dryings, 1.05kg microcrystalline celluloses) are weighed
(grain size is less than or equal to 1 micron), 0.45kg boron phosphates (grain size is less than or equal to 1 micron).
It should be noted that as long as the raw material that this step weighs ensures the organic boron nitrogen combustion inhibitor (contraposition amino nitrile benzene
Boric acid) and fire retarding synergist (microcrystalline cellulose, boron phosphate) mass percent and be less than or equal to 30%, the organic boron
The mass percent of nitrogen combustion inhibitor (contraposition amino nitrile phenyl boric acid) is less than or equal to 15%.
S1c the contraposition amino nitrile phenyl boric acid, microcrystalline cellulose, boron phosphate and the polylactic resin that weigh) are placed in height
Blended under agitation obtains blend composition in fast batch mixer.
S1d) blend composition is injected in Multi-stage heating double screw extruder and carries out melt blending, squeeze out (extrusion temperature
Be 180 DEG C), be granulated, be dry, composite polylactic acid master batch is made.In gained composite polylactic acid master batch, the contraposition amino nitrile benzene boron
Mass percent shared by acid is close to 15%.
S2) polylactic acid is produced using the polylactic resin of a certain amount of composite polylactic acid master batch and equivalent
Composite fibre.
In the present embodiment, is mixed by 50/50 with the polylactic resin with the composite polylactic acid masterbatch of gained, pass through melting
The PLA Composite Fiber is made in the techniques such as spinning-drawing machine spinning, drawing-off and winding.Wherein, hot gas spring temperature is 80 DEG C.
The performance test of PLA Composite Fiber
Weavability：
It is measured according to means of testing commonly used in the prior art, gained PLA Composite Fiber line density is 4.5dtex, is broken
Resistance to spalling 2.9cN/dtex, the surface of the PLA Composite Fiber is smooth, has good weavability.
Anti-flammability：
It is tested according to GB/T5454-1997 (textile combustion performance test oxygen index method), the PLA Composite Fiber
LOI values are 32.5；
Smoke-suppressing：
It is tested according to GB/T16172-2007 (construction material heat release rate test method) using cone calorimetry, this is poly-
The smoke density (SEA) of lactic acid composite fibre reduces 92%.
Performance after washing：
According to GB/T3921.1-1997 (textile color stability tests color fastness to washing experiment) test, the polylactic acid is compound
The reduction of LOI value and smoke density (SEA) of the fiber after 30 washings is no more than 5%.
In conclusion compared with comparative sample, the advantages of implementing the PLA Composite Fiber provided in this embodiment, is：
1, since PLA Composite Fiber described in the present embodiment includes suitable contraposition amino nitrile phenyl boric acid so that described
PLA Composite Fiber not only has efficient flame retardant property but also can effectively inhibit the generation of smog.
2, PLA Composite Fiber described in the present embodiment includes microcrystalline cellulose and a small amount of boron phosphate so that described poly-
After lactic acid composite fibre is lighted once in a while, without apparent molten drop phenomenon, lower section flocking phenomenon on fire is not caused yet.
3, PLA Composite Fiber described in the present embodiment remains to keep every superperformance after the washing of multiple standard.
Embodiment two
The present embodiment provides a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibres and preparation method thereof.
PLA Composite Fiber
PLA Composite Fiber provided in this embodiment and embodiment one difference lies in：The organic boron nitrogen combustion inhibitor is
The contraposition phenyl boric acid (molecular weight 3420, boron content 2.4%) of polyethyleneimine multidigit grafting, the fire retarding synergist are lignin
With the mixture of ammonium polyphosphate.In other words, the PLA Composite Fiber provided in this embodiment is connect by polyethyleneimine multidigit
Contraposition phenyl boric acid, the lignin of branch, ammonium polyphosphate and polylactic resin composition, wherein the polyethyleneimine multidigit grafting
The mass percent for aligning phenyl boric acid is about 6.75%.
The preparation of PLA Composite Fiber
S1) composite polylactic acid mother is produced using a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin
Grain.Wherein, the grain size of the fire retarding synergist is less than or equal to 1 micron.
In the present embodiment, it is specifically divided into following steps：
S1a contraposition phenyl boric acid, lignin, ammonium polyphosphate and the polylactic acid of a certain amount of polyethyleneimine multidigit grafting) are taken
Resin is 24 hours dry in 120 ± 5 DEG C of baking oven.
S1b the contraposition benzene of the polylactic resin of 7.0kg dryings and the polyethyleneimine multidigit grafting of 1.35kg dryings) is weighed
Boric acid, 1.05kg lignin, 0.6kg ammonium polyphosphate.
It should be noted that as long as the raw material that this step weighs ensures the organic boron nitrogen combustion inhibitor, (polyethyleneimine is more
Position grafting contraposition phenyl boric acid) and fire retarding synergist (lignin, ammonium polyphosphate) mass percent and be less than or equal to
30%, the mass percent of the organic boron nitrogen combustion inhibitor (the contraposition phenyl boric acid of polyethyleneimine multidigit grafting) is less than or equal to
15%.
S1c) by the contraposition phenyl boric acid of the polyethyleneimine multidigit weighed grafting, lignin, ammonium polyphosphate and poly- breast
Acid resin is placed in blended under agitation in high speed mixer and obtains blend composition.
S1d) blend composition is injected in Multi-stage heating double screw extruder and carries out melt blending, squeeze out (extrusion temperature
Be 175 DEG C), be granulated, be dry, composite polylactic acid master batch is made.Quality shared by the contraposition phenyl boric acid of polyethyleneimine multidigit grafting
Percentage about 13.5%
S2) polylactic acid is produced using the polylactic resin of a certain amount of composite polylactic acid master batch and equivalent
Composite fibre.
In the present embodiment, is mixed by 50/50 with the polylactic resin with the composite polylactic acid masterbatch of gained, pass through melting
The PLA Composite Fiber is made in the techniques such as spinning-drawing machine spinning, drawing-off and winding.Wherein, hot gas spring temperature is 80 DEG C.
The performance test of PLA Composite Fiber
Weavability：
It is measured according to means of testing commonly used in the prior art, gained PLA Composite Fiber line density is 4.5dtex, is broken
Resistance to spalling 2.5cN/dtex, the surface of the PLA Composite Fiber is smooth, has good weavability.
Anti-flammability：
It is tested according to GB/T5454-1997 (textile combustion performance test oxygen index method), the PLA Composite Fiber
LOI values are 33.2；
Smoke-suppressing：
It is tested according to GB/T16172-2007 (construction material heat release rate test method) using cone calorimetry, this is poly-
The smoke density (SEA) of lactic acid composite fibre reduces 87%.
Performance after washing：
According to GB/T3921.1-1997 (textile color stability tests color fastness to washing experiment) test, the polylactic acid is compound
The reduction of LOI value and smoke density (SEA) of the fiber after 30 washings is no more than 5%.
Described in summary, compared with comparative sample, the PLA Composite Fiber provided in this embodiment has and embodiment one
The identical advantage of the PLA Composite Fiber of offer.
In addition, in terms of anti-flammability, PLA Composite Fiber described in the present embodiment is slightly better than what embodiment one provided
PLA Composite Fiber；PLA Composite Fiber described in the present embodiment is slightly inferior to embodiment one offer in terms of the smoke-suppressing
PLA Composite Fiber.
Embodiment three
The present embodiment provides a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibres and preparation method thereof.
PLA Composite Fiber
PLA Composite Fiber provided in this embodiment and embodiment one difference lies in：The organic boron nitrogen combustion inhibitor is
The contraposition phenyl boric acid (molecular weight 100000, boron content 1.9%) of chitosan multidigit grafting, the fire retarding synergist are starch and plant
The mixture of sour ammonium.In other words, the contraposition benzene that the PLA Composite Fiber provided in this embodiment is grafted by chitosan multidigit
Boric acid, starch, phytic acid ammonium and polylactic resin composition, wherein the quality hundred of the contraposition phenyl boric acid of the chitosan multidigit grafting
Score is about 6.00%.
The preparation of PLA Composite Fiber
S1) composite polylactic acid mother is produced using a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin
Grain.Wherein, the grain size of the fire retarding synergist is less than or equal to 1 micron.
In the present embodiment, it is specifically divided into following steps：
S1a) take contraposition phenyl boric acid, starch, phytic acid ammonium and the polylactic resin of a certain amount of chitosan multidigit grafting in 120
It is 24 hours dry in ± 5 DEG C of baking oven.
S1b the contraposition phenyl boric acid of the polylactic resin of 7.0kg dryings and the chitosan multidigit grafting of 1.2kg dryings) is weighed,
1.15kg starch, 0.65kg phytic acid ammoniums.
It should be noted that as long as the raw material that this step weighs ensures that (chitosan multidigit connects the organic boron nitrogen combustion inhibitor
The contraposition phenyl boric acid of branch) and fire retarding synergist (starch, phytic acid ammonium) mass percent and less than or equal to 30%, it is described to have
The mass percent of machine boron nitrogen combustion inhibitor (the contraposition phenyl boric acid of chitosan multidigit grafting) is less than or equal to 15%.
S1c) contraposition phenyl boric acid, starch, phytic acid ammonium and polylactic resin that the chitosan multidigit weighed is grafted are set
Blended under agitation obtains blend composition in high speed mixer.
S1d) blend composition is injected in Multi-stage heating double screw extruder and carries out melt blending, squeeze out (extrusion temperature
Be 175 DEG C), be granulated, be dry, composite polylactic acid master batch is made.Quality percentage shared by the contraposition phenyl boric acid of chitosan multidigit grafting
Number about 12%.
S2) polylactic acid is produced using the polylactic resin of a certain amount of composite polylactic acid master batch and equivalent
Composite fibre.
In the present embodiment, is mixed by 50/50 with the polylactic resin with the composite polylactic acid masterbatch of gained, pass through melting
The PLA Composite Fiber is made in the techniques such as spinning-drawing machine spinning, drawing-off and winding.Wherein, hot gas spring temperature is 80 DEG C.
The performance test of PLA Composite Fiber
Weavability：
It is measured according to means of testing commonly used in the prior art, gained PLA Composite Fiber line density is 4.5dtex, is broken
Resistance to spalling 3.0cN/dtex, the surface of the PLA Composite Fiber is smooth, has good weavability.
Anti-flammability：
It is tested according to GB/T5454-1997 (textile combustion performance test oxygen index method), the PLA Composite Fiber
LOI values are 30.7；
Smoke-suppressing：
It is tested according to GB/T16172-2007 (construction material heat release rate test method) using cone calorimetry, this is poly-
The smoke density (SEA) of lactic acid composite fibre reduces 81%.
Performance after washing：
According to GB/T3921.1-1997 (textile color stability tests color fastness to washing experiment) test, the polylactic acid is compound
The reduction of LOI value and smoke density (SEA) of the fiber after 30 washings is no more than 5%.
Described in summary, compared with comparative sample, the PLA Composite Fiber provided in this embodiment has and embodiment one
The identical advantage of the PLA Composite Fiber of offer.
In addition, in terms of anti-flammability, PLA Composite Fiber described in the present embodiment is slightly inferior to what embodiment one provided
PLA Composite Fiber；PLA Composite Fiber described in the present embodiment is slightly inferior to embodiment one offer in terms of the smoke-suppressing
PLA Composite Fiber.
The embodiment of the present invention is described above, but the invention is not limited in above-mentioned specific embodiment parties
Formula, the above mentioned embodiment is only schematical, rather than restrictive, and those skilled in the art are in this hair
Under bright enlightenment, without breaking away from the scope protected by the purposes and claims of the present invention, many forms can be also made, this
Within all belonging to the scope of protection of the present invention.
Claims (10)
1. a kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre, which is characterized in that the PLA Composite Fiber is by organic boron
Nitrogen combustion inhibitor, fire retarding synergist and polylactic resin these three components composition.
2. PLA Composite Fiber according to claim 1, which is characterized in that described in the PLA Composite Fiber
The mass percentage of organic boron nitrogen combustion inhibitor is less than or equal to 7.5%.
3. PLA Composite Fiber according to claim 2, which is characterized in that the molecular weight of the organic boron nitrogen combustion inhibitor
For 160-100000.
4. PLA Composite Fiber according to claim 3, which is characterized in that the molecule knot of the organic boron nitrogen combustion inhibitor
Include nitrogen-atoms, boron atom and phenyl ring in structure, wherein boron atom is directly connected by covalent bond with phenyl ring, and the number of boron atom
Quantity of the amount less than nitrogen-atoms.
5. PLA Composite Fiber according to claim 1, which is characterized in that the fire retarding synergist includes natural polymer
Son and phosphorus-containing compound.
6. PLA Composite Fiber according to claim 5, which is characterized in that the natural polymer be selected from cellulose,
Any one in lignin and starch.
7. PLA Composite Fiber according to claim 5, which is characterized in that the phosphorus-containing compound be selected from boron phosphate,
Any one in ammonium polyphosphate and phytic acid ammonium.
8. a kind of preparation method of PLA Composite Fiber as described in claim 1, which is characterized in that include the following steps：
S1) composite polylactic acid master batch is produced using a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin；
S2) to produce the polylactic acid using the polylactic resin of a certain amount of composite polylactic acid master batch and equivalent compound
Fiber.
9. preparation method according to claim 8, which is characterized in that the step S1) include the following steps：
S1a a certain amount of organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin) is taken to be placed in the baking oven of certain temperature
Middle dry a period of time；
S1b) organic boron nitrogen combustion inhibitor, fire retarding synergist and polylactic resin are weighed respectively by certain mass percent, wherein
The mass percent of the organic boron nitrogen combustion inhibitor and fire retarding synergist and be less than or equal to 30%, the organic boron nitrogen is fire-retardant
The mass percent of agent is less than or equal to 15%；
S1c) the organic boron nitrogen combustion inhibitor, fire retarding synergist and the polylactic resin that weigh are placed in high speed mixer and are stirred
Blending obtains blend composition；
S1d) blend composition is injected and carries out melt blending, extrusion, granulation, drying in Multi-stage heating double screw extruder, system
Obtain the composite polylactic acid master batch.
10. preparation method according to claim 9, which is characterized in that the step S1a) in the fire retarding synergist
Grain size be less than or equal to 1 micron.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710054187.7A CN108342788A (en) | 2017-01-22 | 2017-01-22 | A kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710054187.7A CN108342788A (en) | 2017-01-22 | 2017-01-22 | A kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108342788A true CN108342788A (en) | 2018-07-31 |
Family
ID=62962097
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710054187.7A Pending CN108342788A (en) | 2017-01-22 | 2017-01-22 | A kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108342788A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778724A (en) * | 2021-01-04 | 2021-05-11 | 香港理工大学 | Flame-retardant smoke-inhibiting polylactic acid composite material and preparation method thereof |
| CN114855298A (en) * | 2022-04-14 | 2022-08-05 | 东华大学 | Flame-retardant smoke-inhibiting polylactic acid fiber and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101724236A (en) * | 2008-10-24 | 2010-06-09 | 比亚迪股份有限公司 | Polylactic acid flame-retardant material composite, polylactic acid flame-retardant material and preparation method thereof |
| CN103122498A (en) * | 2013-03-19 | 2013-05-29 | 东华大学 | Preparation method of halogen-free flame-retardant polylactic acid fiber |
| KR101350993B1 (en) * | 2013-10-18 | 2014-01-23 | 이재식 | Manufacturing method of pla filament for 3d print and pla filament manufactured thereby |
| CN105440291A (en) * | 2015-12-04 | 2016-03-30 | 沈阳化工大学 | Boron-nitrogen-phosphorus-integrated polymeric type flame retardant and preparing method thereof |
| CN106012085A (en) * | 2016-07-27 | 2016-10-12 | 张蒙 | Polylactic acid fiber fabric for automobile seat cushion |
-
2017
- 2017-01-22 CN CN201710054187.7A patent/CN108342788A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101724236A (en) * | 2008-10-24 | 2010-06-09 | 比亚迪股份有限公司 | Polylactic acid flame-retardant material composite, polylactic acid flame-retardant material and preparation method thereof |
| CN103122498A (en) * | 2013-03-19 | 2013-05-29 | 东华大学 | Preparation method of halogen-free flame-retardant polylactic acid fiber |
| KR101350993B1 (en) * | 2013-10-18 | 2014-01-23 | 이재식 | Manufacturing method of pla filament for 3d print and pla filament manufactured thereby |
| CN105440291A (en) * | 2015-12-04 | 2016-03-30 | 沈阳化工大学 | Boron-nitrogen-phosphorus-integrated polymeric type flame retardant and preparing method thereof |
| CN106012085A (en) * | 2016-07-27 | 2016-10-12 | 张蒙 | Polylactic acid fiber fabric for automobile seat cushion |
Non-Patent Citations (2)
| Title |
|---|
| SHUK YING CHAN等: "一种制备绿色阻燃后整理棉织物的简易方法", 《第一届澳火安全材料科学与工程研讨会》 * |
| 徐鼐: "《通用级聚乳酸的改性与加工成型》", 31 January 2016 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112778724A (en) * | 2021-01-04 | 2021-05-11 | 香港理工大学 | Flame-retardant smoke-inhibiting polylactic acid composite material and preparation method thereof |
| CN114855298A (en) * | 2022-04-14 | 2022-08-05 | 东华大学 | Flame-retardant smoke-inhibiting polylactic acid fiber and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102653890B (en) | Preparation method of highly-spinnable halogen-free flame-retardant nylon fiber | |
| CN101353863B (en) | Method for preparing flame-retardant anti-dripping fibre or fabric and flame-retardant anti-dripping fibre or fabric | |
| CN105133085B (en) | The preparation method of environmental-protection flame-retardant polyester bulk filament | |
| CN103073881B (en) | Nylon composition, preparation method and applications thereof | |
| CN102311639B (en) | High glowing filament flame-retardant glass fiber reinforced polyamide material easy for colour matching and preparation method thereof | |
| CN103160949B (en) | Nanometer inflaming retarding nylon 66 fiber and preparation method thereof | |
| Qin et al. | Construction of flame retardant coating on polyester fabric with ammonium polyphosphate and carbon microspheres | |
| CN104120505A (en) | Inflaming retarding modified PBT (Polybutylene Terephthalate) fiber and preparation method thereof | |
| CN102534855B (en) | Method for preparing halogen-free flame-retarding polyester fibers with durability and droplet resistance | |
| CN114574996B (en) | Flame-retardant composite polyester filament yarn and processing technology thereof | |
| CN108342788A (en) | A kind of flame-retardant smoke inhibition enhanced polylactic acid acid composite fibre and preparation method thereof | |
| CN103484966A (en) | Polyacrylonitrile fiber with flame resistance and preparation method thereof | |
| CN107286603A (en) | Special halogen-free antiflaming polyester master batch of a kind of simulation hairline and preparation method thereof | |
| CN106832581A (en) | A kind of flame-retardant polypropelene resin combination | |
| Zhang et al. | Simultaneous enhancement of mechanical strength and flame retardancy of lyocell fiber via filling fire-resistant cellulose-based derivative | |
| CN110158188A (en) | A kind of high-strength flame-resistant terylene industrial yarn preparation method | |
| CN102400244A (en) | Method for producing flame-retardant melt-drip resistant polyester short fibers | |
| CN101580976B (en) | Preparation method of melt-drip resistant inflaming retarding polyester fiber | |
| CN106609403B (en) | Fiber, fiber master batch and manufacturing method thereof | |
| CN107841136A (en) | A kind of flame-proof glass fibre reinforced plastic PA66 material and its preparation method and application | |
| CN110453499A (en) | Polypropylene flame redardant complex yarn and its product | |
| CN103173888A (en) | Halogen-free flame retardant polyester material and preparation method thereof | |
| CN106498732A (en) | Fire resistance fibre of attachment phospho hetero phenanthrene triazine double-basis compound and preparation method thereof | |
| CN110054809B (en) | Composite flame retardant, preparation method thereof and application thereof in polypropylene | |
| CN113802212B (en) | Flame-retardant fiber, preparation method thereof and flame-retardant fabric |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180731 |
|
| RJ01 | Rejection of invention patent application after publication |