CN109505025A - A kind of anti-fire modified PET fiber and preparation method thereof - Google Patents
A kind of anti-fire modified PET fiber and preparation method thereof Download PDFInfo
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- CN109505025A CN109505025A CN201811423160.1A CN201811423160A CN109505025A CN 109505025 A CN109505025 A CN 109505025A CN 201811423160 A CN201811423160 A CN 201811423160A CN 109505025 A CN109505025 A CN 109505025A
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- flame
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- pet fiber
- retardant
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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
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
Abstract
The present invention relates to fibers and preparation method thereof, and in particular to a kind of flame-retardant modified PET fiber and preparation method thereof.A kind of flame-retardant modified PET fiber, is made of the component comprising following mass parts: 40-45 parts of terephthalic acid (TPA), 35-40 parts of ethylene glycol, 0.5-1 parts of catalyst, 10-15 parts of modified flame-retardant agent, 1-5 parts of antistatic agent, 0.1-0.5 parts of antioxidant, 0.5-1.5 parts of phosphoric acid, 0.5-1 parts of stabilizer.A kind of flame-retardant modified PET fiber of the invention and preparation method thereof, the fiber of preparation is nontoxic, preferable heat resistance and washing fastness, performance are stablized, reached efficiently, safety, low cigarette, nontoxic and UL94 V-0 grade flame retardant effect；Preparation method is simple, easy to operate, easy to control, at low cost, and environmental protection is suitble to scale metaplasia to produce.
Description
Technical field
The present invention relates to fibers and preparation method thereof, and in particular to a kind of flame-retardant modified PET fiber and preparation method thereof.
Background technique
Polyester fiber has the characteristics that intensity is high, elasticity is good, wrinkle resistance is strong, wearability is good and excellent heat resistance.Cause
No matter this is one kind ideal textile material civilian and industrially be widely used.Polyester fiber is currently synthetic fibers
The kind that middle yield is maximum, purposes is most wide, due to its good mechanical performance and tensile property, be widely used dress ornament,
The fields such as industry, good logical transport, ornament materials.But with the expansion of its application field, field is used in certain special dimensions
It closes, such as ornament materials, fire fighting device of military affairs, aviation, communications and transportation, public place of entertainment, hospital etc. etc., then needs to reach certain
Flame-retardancy requirements.According to data at home and abroad introduction, the fire cause of half is related with textile.
Pet fiber, abbreviation PET fiber, is commonly called as terylene, has good mechanical performance, nontoxic nothing
The advantages that taste, wholesomeness be good, oil resistant, choke, cost performance is high, is one of chemical fibre most widely used at present.But PET's
Pole oxygen index (OI) is low, belongs to flammable fiber, so that it has huge security risk in the application.
PET fire-retardant product is competitively all being developed all over the world at present, but existing Flame-retardant PET is often deposited in practical applications
In following problems: some Flame-retardant PETs can produce thick smoke in burning and toxic and harmful gas；Although some Flame-retardant PETs have excellent
Fire-retardant, suppression hood, but material mechanical properties decrease itself is too many, at fine difficult, it is difficult to meet actual operation requirements.
Summary of the invention
In order to solve the above technical problems, the purpose of the present invention is to provide a kind of good flame retardation effects, excellent in mechanical performance
Flame-retardant modified PET fiber and preparation method thereof.
A kind of flame-retardant modified PET fiber, is made of the component comprising following mass parts:
40-45 parts of terephthalic acid (TPA), 35-40 parts of ethylene glycol, 0.5-1 parts of catalyst, 10-15 parts of modified flame-retardant agent, resist it is quiet
Electric agent 1-5 parts, 0.1-0.5 parts of antioxidant, 0.5-1 parts of stabilizer.
Further, catalyst described above is titanate esters and the compounding that antimony oxide 1-3:2-1 in mass ratio is formed
Object.
Further, titanate esters described above are one of tetraethyl titanate, four n-propyl of metatitanic acid, tetra-n-butyl titanate
Or it is several.
Further, modified flame-retardant agent described above is magnesium hydroxide coated silica microballoon, is made as follows
It is standby: (1) to take cetyl trimethylammonium bromide to be scattered in the ethanol water that mass fraction is 30-35%, mass fraction is
1-5%, then sodium hydroxide is added thereto, adjusting pH value is 9-11, in 25 DEG C of stirring 40min under conditions of magnetic agitation；
(2) it weighs mass ratio to be added in step (1) reaction solution for the ethyl orthosilicate and magnesium sulfate of 1:1, mass fraction 1-3%,
React 3-5h；(3) it by sediment centrifugation, washing, is placed in 85-90 DEG C of air dry oven and dries, obtaining partial size is 100-
The powder of 300nm white.
Further, antistatic agent described above is zinc oxide and sodium alkyl sulfonate (1-3) in mass ratio: 1 composition is answered
With object.
Further, above-mentioned antioxidant is Hinered phenols antioxidant 1010 and/or phosphite ester antioxidant 168.
Further, above-mentioned stabilizer is phosphite ester and phosphoric acid, mass ratio 1:1-5.
Further, phosphite ester described above is triphenyl phosphite, in Trimethyl phosphite, three certain herbaceous plants with big flowers ester of phosphorous acid
It is one or more of.
Further, the preparation method of a kind of flame-retardant modified PET fiber, includes the following steps:
(1) modified flame-retardant agent, antistatic agent, ethylene glycol are added in reaction kettle, are stirred at being 55-65 DEG C in temperature
0.5-1h；
(2) terephthalic acid (TPA), catalyst, phosphoric acid are added in the reaction kettle of step (1), increase system temperature to 220-
240 DEG C, react 3-5h；
(3) be added antioxidant, stabilizer, then vacuumize, quickly increase temperature to 260-280 DEG C, polycondensation reaction 3-5h,
When the viscosity of polymer is 0.6-0.9 range, i.e., reaction was completed obtains flame-retardant modified PET polyester；
(4) the antistatic modified PBT polyester for obtaining step (3) carries out melt spinning by screw type spinning machine, cooling
Afterwards, it is oiled, preliminary draft, winding, drawing-off processing, obtains the flame-retardant modified PET fiber that structure is uniform, fiber number is controllable.
Further, step described above (4) spinning temperature is 260-270 DEG C, spinning speed 500-1200m/min,
Stretching and drawing rate is 2-4, and processing temperature is 65-80 DEG C.
Beneficial effects of the present invention:
(1) a kind of flame-retardant modified PET fiber and preparation method thereof of the invention, the modified flame-retardant agent of addition is with super strength
Flame retardant property, contact when fiber kindling can be effectively reduced compared with small particle magnesium hydroxide coated silica microballoon with oxygen
Area, and can have preferable compatibility with polymer melt, improve the mechanical strength of fiber, with the zinc oxide in antistatic agent
With preferable synergistic effect, so that the anti-flammability of fiber is efficient, persistently.
(2) a kind of flame-retardant modified PET fiber and preparation method thereof of the invention, the composite catalyst and compounding of selection are stablized
Agent ensure that system reaction is efficiently gone on smoothly, and in the pyrocondensation stage, there is preferable collaboration to make for phosphoric acid and phosphite ester
With polymer viscosity is improved, product with stable quality.
(3) a kind of flame-retardant modified PET fiber and preparation method thereof of the invention, the fiber of preparation are nontoxic, preferable heat-resisting
Property and washing fastness, performance stablize, reached efficiently, safety, low cigarette, nontoxic and UL94V-0 grade flame retardant effect.
(4) a kind of flame-retardant modified PET fiber and preparation method thereof of the invention, preparation method is simple, easy to operate, easily-controllable
System, at low cost, environmental protection is suitble to scale metaplasia to produce.
Specific embodiment
Presently in connection with embodiment, the present invention is described in further detail.
Embodiment 1
A kind of flame-retardant modified PET fiber, is made of the component comprising following mass parts:
The catalysis of 45 parts of terephthalic acid (TPA), 37 parts of ethylene glycol, tetraethyl titanate and antimony oxide 1:2 in mass ratio composition
What 0.5 part of agent, 15 parts of magnesium hydroxide coated silica microballoon, zinc oxide and sodium alkyl sulfonate 1:1 in mass ratio were formed resists quiet
1 part of electric agent, Hinered phenols antioxidant 1010 and the 1:1 in mass ratio of phosphite ester antioxidant 168 composition 0.5 part of antioxidant,
1 part of stabilizer of Trimethyl phosphite and phosphoric acid 1:3 in mass ratio composition.
Embodiment 2-4, comparative example 1-3 are substantially the same manner as Example 1, difference such as table 1.
Table 1
Modified flame-retardant agent described in embodiment 1-4 and comparative example 1-5 is magnesium hydroxide coated silica microballoon, by such as
The preparation of lower section method: (1) cetyl trimethylammonium bromide is taken to be scattered in the ethanol water that mass fraction is 30-35%, matter
Amount score is 1-5%, then sodium hydroxide is added thereto, and adjusting pH value is 9-11, is stirred under conditions of magnetic agitation in 25 DEG C
Mix 40min；(2) it weighs mass ratio to be added in step (1) reaction solution for the ethyl orthosilicate and magnesium sulfate of 1:1, mass fraction
For 1-3%, 3-5h is reacted；(3) it by sediment centrifugation, washing, is placed in 85-90 DEG C of air dry oven and dries, obtain partial size
For the powder of 100-300nm white.
A kind of preparation method of flame-retardant modified PET fiber, includes the following steps: described in embodiment 1-4 and comparative example 1-5
(1) modified flame-retardant agent, antistatic agent, ethylene glycol are added in reaction kettle, are stirred at being 55-65 DEG C in temperature
0.5-1h；
(2) terephthalic acid (TPA), catalyst, phosphoric acid are added in the reaction kettle of step (1), increase system temperature to 220-
240 DEG C, react 3-5h；
(3) be added antioxidant, stabilizer, then vacuumize, quickly increase temperature to 260-280 DEG C, polycondensation reaction 3-5h,
When the viscosity of polymer is 0.6-0.9 range, i.e., reaction was completed obtains flame-retardant modified PET polyester；
(4) the antistatic modified PBT polyester for obtaining step (3) carries out melt spinning by screw type spinning machine, cooling
Afterwards, it is oiled, preliminary draft, winding, drawing-off processing, obtains the flame-retardant modified PET fiber that structure is uniform, fiber number is controllable, wherein
Spinning molten temperature is 260-270 DEG C, spinning speed 500-1200m/min, and stretching and drawing rate is 2-4, processing temperature 65-
80℃。
By fibre property such as table 2 obtained by above-described embodiment 1-4 and comparative example 1-5
Table 2
From table 2 it can be seen that PET fiber intensity made from embodiment 1-4 is higher, flame retardant effect reaches UL94V-0 etc.
Grade, and comparative example 1-5 is due to component parameter variation, fibre property reduction, flame retardant effect variation.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.
Claims (10)
1. a kind of flame-retardant modified PET fiber, it is characterised in that: be made of the component comprising following mass parts:
It is 40-45 parts of terephthalic acid (TPA), 35-40 parts of ethylene glycol, 0.5-1 parts of catalyst, 10-15 parts of modified flame-retardant agent, antistatic
1-5 parts of agent, 0.1-0.5 parts of antioxidant, 0.5-1 parts of stabilizer.
2. a kind of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the catalyst be titanate esters and
The compound of antimony oxide 1-3:2-1 in mass ratio composition.
3. a kind of flame-retardant modified PET fiber as claimed in claim 2, which is characterized in that the titanate esters are metatitanic acid tetrem
One or more of ester, four n-propyl of metatitanic acid, tetra-n-butyl titanate.
4. a kind of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the modified flame-retardant agent is hydrogen-oxygen
Change magnesium coated silica microballoon, is prepared as follows: (1) taking cetyl trimethylammonium bromide to be scattered in mass fraction
For in the ethanol water of 30-35%, the mass fraction of cetyl trimethylammonium bromide is 1-5%, then hydrogen-oxygen is added thereto
Change sodium, adjusting pH value is 9-11, in 25 DEG C of 40 min of stirring under conditions of magnetic agitation；(2) weighing mass ratio is 1:1's
Ethyl orthosilicate and magnesium sulfate are added in step (1) reaction solution, and the mass fraction of ethyl orthosilicate and magnesium sulfate is 1-3%, instead
Answer 3-5 h；(3) it by sediment centrifugation, washing, is placed in 85-90 DEG C of air dry oven and dries, obtaining partial size is 100-
The powder of 300nm white.
5. a kind of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the antistatic agent is zinc oxide
With the compound of sodium alkyl sulfonate 1-3:1 in mass ratio composition.
6. a kind of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the antioxidant is Hinered phenols
Antioxidant 1010 and/or phosphite ester antioxidant 168, preferably Hinered phenols antioxidant 1010 and/or phosphorous acid esters
The ratio of irgasfos 168 is 1:1.
7. a kind of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the stabilizer is phosphite ester
With phosphoric acid, mass ratio 1:1-5.
8. a kind of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the phosphite ester is phosphorous acid
One or more of triphenylmethyl methacrylate, Trimethyl phosphite, three certain herbaceous plants with big flowers ester of phosphorous acid.
9. a kind of preparation method of such as described in any item flame-retardant modified PET fiber of claim 1-8, which is characterized in that including
Following steps:
(1) modified flame-retardant agent, antistatic agent, ethylene glycol are added in reaction kettle, stir 0.5- at being 55-65 DEG C in temperature
1h；
(2) terephthalic acid (TPA), catalyst, phosphoric acid are added in the reaction kettle of step (1), increase system temperature to 220-240
DEG C, react 3-5h；
(3) antioxidant, stabilizer is added, then vacuumizes, quickly increases temperature to 260-280 DEG C, polycondensation reaction 3-5h, when poly-
When the viscosity for closing object is 0.6-0.9 range, i.e., reaction was completed obtains flame-retardant modified PET polyester；
(4) the antistatic modified PBT polyester for obtaining step (3) carries out melt spinning by screw type spinning machine, after cooling, into
Row oils, preliminary draft, winding, drawing-off processing, obtains the flame-retardant modified PET fiber that structure is uniform, fiber number is controllable.
10. the preparation method of flame-retardant modified PET fiber as described in claim 1, which is characterized in that the step (4) is spun
Silk temperature is 260-270 DEG C, spinning speed 500-1200m/min, and stretching and drawing rate is 2-4, and processing temperature is 65-80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811423160.1A CN109505025A (en) | 2018-11-27 | 2018-11-27 | A kind of anti-fire modified PET fiber and preparation method thereof |
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| CN201811423160.1A CN109505025A (en) | 2018-11-27 | 2018-11-27 | A kind of anti-fire modified PET fiber and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117624573A (en) * | 2024-01-25 | 2024-03-01 | 江苏恒力化纤股份有限公司 | Flame-retardant polyester with homogeneously dispersed silicon dioxide, and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117624573A (en) * | 2024-01-25 | 2024-03-01 | 江苏恒力化纤股份有限公司 | Flame-retardant polyester with homogeneously dispersed silicon dioxide, and preparation method and application thereof |
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