CN109503946A - A kind of plant source polypropylene fibre master batch and preparation method thereof - Google Patents
A kind of plant source polypropylene fibre master batch and preparation method thereof Download PDFInfo
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- CN109503946A CN109503946A CN201811457135.5A CN201811457135A CN109503946A CN 109503946 A CN109503946 A CN 109503946A CN 201811457135 A CN201811457135 A CN 201811457135A CN 109503946 A CN109503946 A CN 109503946A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- 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
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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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- 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
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/12—Applications used for fibers
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Abstract
The present invention provides a kind of plant source polypropylene fibre master batch, and the plant source polypropylene fibre master batch is polypropylene fibre master batch and modified honeysuckle powder blended melting preparation；The mass ratio of the polypropylene fibre master batch and the modified honeysuckle powder is 85:15；The present invention also provides the preparation methods of above-mentioned cellulose fibre；Plant source polypropylene fibre master batch prepared by the present invention, regular shape, no even grain, no clast, particle size uniformity 95.8-99.1%, oxygen index (OI) (OI) is 29-30；Fiber obtained, line density deviation ratio is 0.7-1.2%, and length variation rate is 0.01-0.06%, breaking strength 7.9-8.3cN/dtex, elongation at break 25.8-30.4%, fault 2.7-2.8mg/100g, the burning time of flame retardant property is 9.4-8.5s, combustion rating V-1；Flame retardant effect is lasting after repeatedly washing, and stablizes.
Description
Technical field
The present invention relates to a kind of plant source polypropylene fibre master batches and preparation method thereof, belong to fiber master batch preparation field.
Background technique
Polypropylene fibre master batch refers to the basic pellet of manufacture polypropylene fiber, with physical chemistry such as certain shape, partial sizes
Matter.Polypropylene fiber is an important species in synthetic fibers, is the product name of China's polyester fiber, and polypropylene fibre has density
The harmonious good, advantages such as price is low of small, nontoxic, corrosion-resistant, mechanics, are a kind of extensive materials of application field.But due to manufacture
Polypropylene of polypropylene fibre itself poor flame retardant properties, to limit it in the application in the fields such as motor, flexible circuit board, electric appliance.
Plant in nature, such as wormwood, folium isatidis, peppermint, honeysuckle etc. plant, due to its own peculiar feature
And ingredient, it is welcome by the technology fan of fiber art, application range is also increasingly wider.
The patent of Publication No. CN107938008A discloses a kind of polypropylene spinning Masterbatch, solves polypropylene spinning process
In the production technology as caused by Masterbatch quality problems, product quality problem, specially solution dyestuff dispersion be not easy to manipulate, wink
Between bond or retain the serious technical problem of uniform sex differernce dispersed between a large amount of fecula and every pot of material.
Application No. is the Chinese patents of CN97105683.8 to disclose a kind of Perpetural polypropylene fiber antistatic master granule, it is will to spin
The rheological characteristic of silk melt improves, and spinning technique is easy to grasp, and causes not feed caused by realizing after addition antistatic agent, can not
The technical issues of spinning；
Publication number CN102219957 discloses a kind of functional masterbatch of halogen-free intumescent flame retardant and preparation method thereof, and the function is female
Halogen-free expansion fire retardant in grain composition is phosphorus-nitrogen expanding fire retardant, and matrix is polyolefin resin.But fire-retardant master granule
Although the dispersibility in matrix resin is good, in the preparation process of fire-retardant master granule, it is easy to appear fire retardant and is not easy to disperse
The problem of, cause the flame retardant effect of fire-retardant master granule poor.
In summary the fiber of the production technology of disclosed polypropylene fibre master batch, existing plant source polypropylene fibre master batch and its preparation,
It has the disadvantage that
(1) the plant source polypropylene fibre master batch uniformity is poor, easily connects grain, and oxygen index (OI) is low；
(2) the fiber bad mechanical property that is prepared by plant source master batch, fault is high, the ultimate strength coefficient of variation is big, flame retardant property drop
It is low；
(3) after repeatedly washing, every mechanical performance reduces serious the fiber prepared by plant source master batch；
(4) fabric as made by plant source master batch fiber, pilling fluffing resistant grade are low.
Summary of the invention
The present invention in order to solve the above technical problems, in view of the deficiencies of the prior art, it is female to provide a kind of plant source polypropylene fibre
Grain and preparation method thereof, to realize following goal of the invention:
(1) the honeysuckle plant source polypropylene fibre master batch particle of 1-3 of embodiment of the present invention preparation is uniform, regular shape, particle surface profit
Pool, no even grain, no clast, honeysuckle plant source polypropylene fibre master batch particle size uniformity are 95.8-99.1%, and oxygen index (OI) (OI) is 29-
30；
(2) 3.2dtex*62mm honeysuckle plant source polypropylene fibre master batch made from honeysuckle plant source polypropylene fibre master batch prepared by the present invention
Fiber product, line density deviation ratio are 0.7-1.2%, and length variation rate is 0.01-0.06%, breaking strength 7.9-8.3cN/
Dtex, elongation at break 25.8-30.4%, fault 2.7-2.8mg/100g, the ultimate strength coefficient of variation (CV) 6.5-6.8%,
Excellent fireproof performance, burning time 9.4-8.5s, combustion rating V-1.
(3) 3.2dtex*62mm honeysuckle plant source polypropylene fibre made from honeysuckle plant source polypropylene fibre master batch prepared by the present invention
Master batch fiber product, after repeatedly washing, every mechanical performance is hardly reduced, and after washing 50 times, breaking strength is
7.7-8.4cN/dtex, elongation at break 32.6-35.1%, combustion rating are V-1 grades；After washing 100 times, breaking strength is
6.8-7.6cN/dtex, elongation at break 35.5-38.1%, combustion rating are V-1 grades.
(4) fabric made by the polypropylene fiber of polypropylene fibre master batch preparation in honeysuckle plant source of the present invention, pilling fluffing resistant performance
Good, scared slight pilling, or even slightly scared no pilling, pilling fluffing resistant grade are not less than 4 grades.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:
A kind of plant source polypropylene fibre master batch is prepared by polypropylene fibre master batch and modified honeysuckle powder blended melting；The polypropylene fibre master batch
Mass ratio with the modified honeysuckle powder is 85:15.
It is further improvement to above-mentioned technical proposal below:
The plant source polypropylene fibre master batch, particle is uniform, regular shape, and particle surface is moist, no even grain, no clast, and honeysuckle is planted
Material resource polypropylene fibre master batch particle size uniformity is 95.8-99.1%, and oxygen index (OI) (OI) is 29-30.
Fiber product made from the plant source polypropylene fibre master batch, line density deviation ratio are 0.7-1.2%, and length variation rate is
0.01-0.06%, breaking strength 7.9-8.3cN/dtex, elongation at break 25.8-30.4%, fault 2.7-2.8mg/
100g, the ultimate strength coefficient of variation (CV) 6.5-6.8%, excellent fireproof performance, burning time 9.4-8.5s, combustion rating are
V-1。
A kind of preparation method of plant source polypropylene fibre master batch, the preparation method includes the preparation of modified honeysuckle powder, described
The preparation of modified honeysuckle powder includes: the selection of (1) raw material
Honeysuckle powder is selected, as the plant source raw material of the present embodiment, the honeysuckle powder, 100% crosses 10000 meshes, appearance powder
End is loose, without agglomeration, color: with the intrinsic color of the product, and uniformity；Smell is uniform；Active constituent content >=
98%, chlorogenic acid content 16.5%, moisture≤5%, total plate count < 100cfu/g, salmonella and Escherichia coli must not be examined
Out, the shelf-life is 18 months.
The preparation of the modified honeysuckle powder includes: that (2) prepare modified honeysuckle powder:
After 50 parts of honeysuckle powders are mixed with the starch of 15-20 parts of chitin and 4-6 part, adjusted after pH is 7-8 with sodium carbonate,
50-70 parts of deionized waters are added and are heated to 51-62 DEG C of mixing 30min, are evaporated under reduced pressure 0.5-1 hours after gains are shaken up
Afterwards, it is then dissolved in 40-60 parts of deionized waters, 10-20 parts of acrylic acid is added after semi-permeable membrane constantly washes 0.5-8 hours and put
Enter in mixer after mixing 1.1-1.6 hours, naturally dry is pulverized, crushed, and obtains modified honeysuckle powder.
Prepared modification honeysuckle powder, compatibility is good, mesh number be 10000 mesh, density 1.08-1.25g/cm3, apparently
Viscosity 30-50mPa.s, honeysuckle content of cellulose are 20.7-26.0%, and the shelf-life is 48 months.
The preparation method of the plant source polypropylene fibre master batch, the preparation including step 2, polypropylene fibre master batch:
Acrylic resin is heated to melting, temperature is 195-210 DEG C, sequentially adds ultraviolet light into the acrylic resin of melting
Protective agent, high activity phosphate LYCO-P08, di-t-butyl peroxide, filler, stir 5 under the revolving speed of 600rad/min
Minute, it is sufficiently mixed each component uniformly, then keeps the BUSS within the scope of 195-210 DEG C of temperature to be kneaded in said mixture material
Unit (model MKD-30), extruding pelletization under conditions of keeping vacuum degree -0.02MPa, obtains polypropylene fibre master batch.
The filler is kaolin powder, the talcum powder, vermiculite being activated through silane coupling agent or titanate coupling agent
Any one of powder, six ring mountain flours, glass microballoon appoint several mixtures.
The ultra-violet protecting agent is GW-508 and light stabilizer UV-292, mass ratio 2:5.
The high activity phosphate LYCO-P08, acid value 10-45mgKOH/g, content of inorganic phosphorus 1.25%, total phosphorus content
8.95%。
The preparation method of the plant source polypropylene fibre master batch, including step 3, addition reaction promoter:
The reaction promoter of 2.6-3.2% is added into modified honeysuckle powder, is heated up to 40-50 DEG C, is stirred with the speed of 900rad/min
It mixes, is uniformly mixed.
The reaction promoter, is made of raw material from the following weight: 3,4- 2 parts of dimethyl -3,4- diphenyl hexanes, surface
2 parts of hardening anti-wear agent T801,3 parts of adipic dihydrazide, 3 parts of epoxychloropropane, 2 parts of defoaming agent BYK025, poly- carbonization two are sub-
4 parts of amine, 2.5 parts of zinc hydroxide.
The adipic dihydrazide, active constituent content 99.2%, CAS number is 1071-93-8.
The polycarbodiimide, the yellowish liquid of viscosity, density (25 DEG C) 1.08g/cm3, fusing point < 5 DEG C, viscosity (40
DEG C) it is 400-700 mPas.
The preparation method of the plant source polypropylene fibre master batch, the preparation including step 4, honeysuckle plant source polypropylene fibre master batch:
Polypropylene fibre master batch is melted at 198 DEG C, 4-8min is stirred with the speed of 800rad/min, changing containing reaction promoter is added
Property honeysuckle powder, inorganic fire retardants and organic titanium cross-linking agent Tyzor371, continue to stir 15min with the speed of 800rad/min,
Cross-linking reaction is carried out, product is obtained.
The mass ratio of the polypropylene fibre master batch and the modified honeysuckle powder is 85:15.
The additive amount of the organic titanium cross-linking agent Tyzor371 is the modification honeysuckle powder gross mass containing reaction promoter
0.1%, the additive amount of the inorganic fire retardants is the 6.5% of polypropylene fibre master batch quality.
The inorganic fire retardants is made of red phosphorus, antimony oxide, zinc borate, acrylic resin, mass ratio 6:1:3:
50。
After above-mentioned product is packed into double screw extruder melting extrusion cooling, it is granulated through pelletizer, obtains honeysuckle plant source
Polypropylene fibre master batch.
Wherein, the melting temperature of double screw extruder is 182-245 DEG C, engine speed 800-900rad/min, feeding
Revolving speed is 500-1000rad/min, and the revolving speed of pelletizer is 900-1100rad/min.
The preparation method of the fibre as made by the plant source polypropylene fibre master batch further includes step 5, spinning
(3.2dtex*62mm):
Melt extruded machine temperature is set as 167 °C, by above-mentioned honeysuckle plant source polypropylene fibre master batch through metering pump after temperature is stablized
It is added after metering, continues to be heated to melt completely, molten mass is subjected to melt spinning via spinneret orifice, using leading for the first time
It stretches, second of drawing-off, third time drawing-off, sizing, winding and be formed again, obtain polypropylene fiber.
Wherein, spinneret orifice surface roughness Ra≤0.2 μm, surface static contact angle WCA >=85 °.
First time drawing temperature is 85-93 DEG C, and second of drawing temperature is 95-102 DEG C, and third time drawing temperature is 105-
115℃。
Using technical solution of the present invention, the beneficial effect of acquisition is:
(1) by being detected to honeysuckle plant source polypropylene fibre master batch prepared by above-described embodiment 1-3, obtained honeysuckle
Plant source polypropylene fibre master batch, particle is uniform, regular shape, and particle surface is moist, no even grain, no clast, honeysuckle plant source polypropylene fibre
Master batch particle size uniformity is 95.8-99.1%, and oxygen index (OI) (OI) is 29-30；
(2) 3.2dtex*62mm honeysuckle plant source polypropylene fibre master batch made from honeysuckle plant source polypropylene fibre master batch prepared by the present invention
Fiber product, line density deviation ratio are 0.7-1.2%, and length variation rate is 0.01-0.06%, breaking strength 7.9-8.3cN/
Dtex, elongation at break 25.8-30.4%, fault 2.7-2.8mg/100g, the ultimate strength coefficient of variation (CV) 6.5-6.8%,
Excellent fireproof performance, burning time 9.4-8.5s, combustion rating V-1.
(3) 3.2dtex*62mm honeysuckle plant source polypropylene fibre made from honeysuckle plant source polypropylene fibre master batch prepared by the present invention
Master batch fiber product, after repeatedly washing, every mechanical performance is hardly reduced, and after washing 50 times, breaking strength is
7.7-8.4cN/dtex, elongation at break 32.6-35.1%, combustion rating are V-1 grades；After washing 100 times, breaking strength is
6.8-7.6cN/dtex, elongation at break 35.5-38.1%, combustion rating are V-1 grades.
(4) fabric made by the polypropylene fiber of polypropylene fibre master batch preparation in honeysuckle plant source of the present invention, pilling fluffing resistant performance
Good, scared slight pilling, or even slightly scared no pilling, pilling fluffing resistant grade are not less than 4 grades.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
A kind of preparation method of the honeysuckle plant source polypropylene fibre master batch of embodiment 1
The preparation of step 1, modified honeysuckle powder
(1) selection of raw material
Honeysuckle powder is selected, as the plant source raw material of the present embodiment, the honeysuckle powder, 100% crosses 10000 meshes, appearance powder
End is loose, without agglomeration, color: with the intrinsic color of the product, and uniformity；Smell is uniform；Active constituent content >=
98%, chlorogenic acid content 16.5%, moisture≤5%, total plate count < 100cfu/g, salmonella and Escherichia coli must not be examined
Out, the shelf-life is 18 months.
(2) modified honeysuckle powder is prepared
After 50 parts of honeysuckle powders are mixed with 15 parts of chitin and 4 parts of starch, after being 7.1 with sodium carbonate adjusting pH, it is added
50 parts of deionized waters are simultaneously heated to 51 DEG C of mixing 30min and are then dissolved in 40 after being evaporated under reduced pressure 0.5 hour after shaking up gains
In part deionized water, 10 parts of acrylic acid are added after semi-permeable membrane constantly washes 0.8 hour and are put into mixing 1.0 hours in mixer
Afterwards, naturally dry, pulverize, crush, obtain modified honeysuckle powder；
Prepared modification honeysuckle powder, compatibility is good, and mesh number is 10000 mesh, density 1.08-1.25g/cm3, apparent viscosity
30-50mPa.s, honeysuckle content of cellulose are 20.7-26.0%, and the shelf-life is 48 months.
The preparation of step 2, polypropylene fibre master batch
Acrylic resin is heated to melting, temperature is 195 DEG C, sequentially adds ultraviolet protection into the acrylic resin of melting
Agent, high activity phosphate LYCO-P08, di-t-butyl peroxide, filler are stirred 5 minutes under the revolving speed of 600rad/min,
It is sufficiently mixed each component uniformly, then keeps the BUSS within the scope of 195-198 DEG C of temperature to be kneaded unit in said mixture material
(model MKD-30), extruding pelletization under conditions of keeping vacuum degree -0.02MPa, obtains polypropylene fibre master batch.
The filler is kaolin powder, the talcum powder, vermiculite being activated through silane coupling agent or titanate coupling agent
Any one of powder, six ring mountain flours, glass microballoon appoint several mixtures；
The ultra-violet protecting agent is GW-508 and light stabilizer UV-292, mass ratio 2:5；
The high activity phosphate LYCO-P08, acid value 10-45mgKOH/g, content of inorganic phosphorus 1.25%, total phosphorus content 8.95%.
Reaction promoter is added in step 3
2.5% reaction promoter is added into modified honeysuckle powder, is heated up to 40 DEG C, is stirred with the speed of 900rad/min, mixing
Uniformly.
The reaction promoter, is made of raw material from the following weight: 3,4- 2 parts of dimethyl -3,4- diphenyl hexanes, surface
2 parts of hardening anti-wear agent T801,3 parts of adipic dihydrazide, 3 parts of epoxychloropropane, 2 parts of defoaming agent BYK025, poly- carbonization two are sub-
4 parts of amine, 2.5 parts of zinc hydroxide.
The adipic dihydrazide, active constituent content 99.2%, CAS number is 1071-93-8；
The polycarbodiimide, the yellowish liquid of viscosity, density (25 DEG C) 1.08g/cm3, fusing point < 5 DEG C, viscosity (40 DEG C) are
400-700 mPas。
The preparation of step 4, honeysuckle plant source polypropylene fibre master batch
Polypropylene fibre master batch is melted at 198 DEG C, 4min is stirred with the speed of 800rad/min, the modification containing reaction promoter is added
Honeysuckle powder, inorganic fire retardants and organic titanium cross-linking agent Tyzor371 continue to stir 15min with the speed of 800rad/min, into
Row cross-linking reaction, obtains product.
The mass ratio of the polypropylene fibre master batch and the modified honeysuckle powder is 85:15；
The additive amount of the organic titanium cross-linking agent Tyzor371 is 0.1% of the modification honeysuckle powder gross mass containing reaction promoter,
The additive amount of the inorganic fire retardants is the 6.5% of polypropylene fibre master batch quality；
The inorganic fire retardants is made of red phosphorus, antimony oxide, zinc borate, acrylic resin, mass ratio 6:1:3:50.
After above-mentioned product is packed into double screw extruder melting extrusion cooling, it is granulated through pelletizer, obtains honeysuckle plant source
Polypropylene fibre master batch.
Wherein, the melting temperature of double screw extruder is 182-245 DEG C, engine speed 800rad/min, feeding revolving speed
For 500rad/min, the revolving speed of pelletizer is 900rad/min.
Step 5, spinning (3.2dtex*62mm)
Melt extruded machine temperature is set as 167 °C, by above-mentioned honeysuckle plant source polypropylene fibre master batch through metering pump after temperature is stablized
It is added after metering, continues to be heated to melt completely, molten mass is subjected to melt spinning via spinneret orifice, using leading for the first time
It stretches, second of drawing-off, third time drawing-off, sizing, winding and be formed again, obtain polypropylene fiber；
Wherein, spinneret orifice surface roughness Ra≤0.2 μm, surface static contact angle WCA >=85 °；
First time drawing temperature is 85 DEG C, and second of drawing temperature is 95 DEG C, and third time drawing temperature is 105 DEG C.
A kind of preparation method of the honeysuckle plant source polypropylene fibre master batch of embodiment 2
The preparation of step 1, modified honeysuckle powder
(1) selection of raw material
Honeysuckle powder is selected, as the plant source raw material of the present embodiment, the honeysuckle powder, 100% crosses 10000 meshes, appearance powder
End is loose, without agglomeration, color: with the intrinsic color of the product, and uniformity；Smell is uniform；Active constituent content >=
98%, chlorogenic acid content 16.5%, moisture≤5%, total plate count < 100cfu/g, salmonella and Escherichia coli must not be examined
Out, the shelf-life is 18 months.
(2) modified honeysuckle powder is prepared
After 50 parts of honeysuckle powders are mixed with 16 parts of chitin and 5 parts of starch, after being 7.5 with sodium carbonate adjusting pH, it is added
60 parts of deionized waters are simultaneously heated to 56 DEG C of mixing 32min and are then dissolved in 50 after being evaporated under reduced pressure 0.8 hour after shaking up gains
In part deionized water, 15 parts of acrylic acid are added after semi-permeable membrane constantly washes 3.5 hours and are put into mixing 1.4 hours in mixer
Afterwards, naturally dry, pulverize, crush, obtain modified honeysuckle powder；
Prepared modification honeysuckle powder, compatibility is good, and mesh number is 10000 mesh, density 1.08-1.25g/cm3, apparent viscosity
30-50mPa.s, honeysuckle content of cellulose are 20.7-26.0%, and the shelf-life is 48 months.
The preparation of step 2, polypropylene fibre master batch
Acrylic resin is heated to melting, temperature is 204 DEG C, sequentially adds ultraviolet protection into the acrylic resin of melting
Agent, high activity phosphate LYCO-P08, di-t-butyl peroxide, filler are stirred 5 minutes under the revolving speed of 600rad/min,
It is sufficiently mixed each component uniformly, then keeps the BUSS within the scope of 197-202 DEG C of temperature to be kneaded unit in said mixture material
(model MKD-30), extruding pelletization under conditions of keeping vacuum degree -0.02MPa, obtains polypropylene fibre master batch.
The filler is kaolin powder, the talcum powder, vermiculite being activated through silane coupling agent or titanate coupling agent
Any one of powder, six ring mountain flours, glass microballoon appoint several mixtures；
The ultra-violet protecting agent is GW-508 and light stabilizer UV-292, mass ratio 2:5；
The high activity phosphate LYCO-P08, acid value 10-45mgKOH/g, content of inorganic phosphorus 1.25%, total phosphorus content 8.95%.
Reaction promoter is added in step 3
2.9% reaction promoter is added into modified honeysuckle powder, is heated up to 43 DEG C, is stirred with the speed of 900rad/min, mixing
Uniformly.
The reaction promoter, is made of raw material from the following weight: 3,4- 2 parts of dimethyl -3,4- diphenyl hexanes, surface
2 parts of hardening anti-wear agent T801,3 parts of adipic dihydrazide, 3 parts of epoxychloropropane, 2 parts of defoaming agent BYK025, poly- carbonization two are sub-
4 parts of amine, 2.5 parts of zinc hydroxide.
The adipic dihydrazide, active constituent content 99.2%, CAS number is 1071-93-8；
The polycarbodiimide, the yellowish liquid of viscosity, density (25 DEG C) 1.08g/cm3, fusing point < 5 DEG C, viscosity (40 DEG C) are
400-700 mPas。
The preparation of step 4, honeysuckle plant source polypropylene fibre master batch
Polypropylene fibre master batch is melted at 198 DEG C, 6min is stirred with the speed of 800rad/min, the modification containing reaction promoter is added
Honeysuckle powder, inorganic fire retardants and organic titanium cross-linking agent Tyzor371 continue to stir 15min with the speed of 800rad/min, into
Row cross-linking reaction, obtains product.
The mass ratio of the polypropylene fibre master batch and the modified honeysuckle powder is 85:15；
The additive amount of the organic titanium cross-linking agent Tyzor371 is 0.1% of the modification honeysuckle powder gross mass containing reaction promoter,
The additive amount of the inorganic fire retardants is the 6.5% of polypropylene fibre master batch quality；
The inorganic fire retardants is made of red phosphorus, antimony oxide, zinc borate, acrylic resin, mass ratio 6:1:3:50.
After above-mentioned product is packed into double screw extruder melting extrusion cooling, it is granulated through pelletizer, obtains honeysuckle plant source
Polypropylene fibre master batch.
Wherein, the melting temperature of double screw extruder is 182-245 DEG C, engine speed 850rad/min, feeding revolving speed
For 780rad/min, the revolving speed of pelletizer is 1020rad/min.
Step 5, spinning (3.2dtex*62mm)
Melt extruded machine temperature is set as 167 °C, by above-mentioned honeysuckle plant source polypropylene fibre master batch through metering pump after temperature is stablized
It is added after metering, continues to be heated to melt completely, molten mass is subjected to melt spinning via spinneret orifice, using leading for the first time
It stretches, second of drawing-off, third time drawing-off, sizing, winding and be formed again, obtain polypropylene fiber；
Wherein, spinneret orifice surface roughness Ra≤0.2 μm, surface static contact angle WCA >=85 °；
First time drawing temperature is 90 DEG C, and second of drawing temperature is 99 DEG C, and third time drawing temperature is 109 DEG C.
A kind of preparation method of the honeysuckle plant source polypropylene fibre master batch of embodiment 3
The preparation of step 1, modified honeysuckle powder
(1) selection of raw material
Honeysuckle powder is selected, as the plant source raw material of the present embodiment, the honeysuckle powder, 100% crosses 10000 meshes, appearance powder
End is loose, without agglomeration, color: with the intrinsic color of the product, and uniformity；Smell is uniform；Active constituent content >=
98%, chlorogenic acid content 16.5%, moisture≤5%, total plate count < 100cfu/g, salmonella and Escherichia coli must not be examined
Out, the shelf-life is 18 months.
(2) modified honeysuckle powder is prepared
After 50 parts of honeysuckle powders are mixed with 20 parts of chitin and 6 parts of starch, after being 8 with sodium carbonate adjusting pH, it is added 70
Part deionized water is simultaneously heated to 62 DEG C of mixing 30min and is then dissolved in 60 parts after being evaporated under reduced pressure 1 hour after shaking up gains and goes
In ionized water, 20 parts of acrylic acid are added after semi-permeable membrane constantly washes 8 hours and are put into mixer after mixing 1.6 hours, from
It so dries, pulverize, crush, obtain modified honeysuckle powder；
Prepared modification honeysuckle powder, compatibility is good, and mesh number is 10000 mesh, density 1.08-1.25g/cm3, apparent viscosity
30-50mPa.s, honeysuckle content of cellulose are 20.7-26.0%, and the shelf-life is 48 months.
The preparation of step 2, polypropylene fibre master batch
Acrylic resin is heated to melting, temperature is 209 DEG C, sequentially adds ultraviolet protection into the acrylic resin of melting
Agent, high activity phosphate LYCO-P08, di-t-butyl peroxide, filler are stirred 5 minutes under the revolving speed of 600rad/min,
It is sufficiently mixed each component uniformly, then keeps the BUSS within the scope of 204-210 DEG C of temperature to be kneaded unit in said mixture material
(model MKD-30), extruding pelletization under conditions of keeping vacuum degree -0.02MPa, obtains polypropylene fibre master batch.
The filler is kaolin powder, the talcum powder, vermiculite being activated through silane coupling agent or titanate coupling agent
Any one of powder, six ring mountain flours, glass microballoon appoint several mixtures；
The ultra-violet protecting agent is GW-508 and light stabilizer UV-292, mass ratio 2:5；
The high activity phosphate LYCO-P08, acid value 10-45mgKOH/g, content of inorganic phosphorus 1.25%, total phosphorus content 8.95%.
Reaction promoter is added in step 3
3.2% reaction promoter is added into modified honeysuckle powder, is heated up to 50 DEG C, is stirred with the speed of 900rad/min, mixing
Uniformly.
The reaction promoter, is made of raw material from the following weight: 3,4- 2 parts of dimethyl -3,4- diphenyl hexanes, surface
2 parts of hardening anti-wear agent T801,3 parts of adipic dihydrazide, 3 parts of epoxychloropropane, 2 parts of defoaming agent BYK025, poly- carbonization two are sub-
4 parts of amine, 2.5 parts of zinc hydroxide.
The adipic dihydrazide, active constituent content 99.2%, CAS number is 1071-93-8；
The polycarbodiimide, the yellowish liquid of viscosity, density (25 DEG C) 1.08g/cm3, fusing point < 5 DEG C, viscosity (40 DEG C) are
400-700 mPas。
The preparation of step 4, honeysuckle plant source polypropylene fibre master batch
Polypropylene fibre master batch is melted at 198 DEG C, 4-8min is stirred with the speed of 800rad/min, changing containing reaction promoter is added
Property honeysuckle powder, inorganic fire retardants and organic titanium cross-linking agent Tyzor371, continue to stir 15min with the speed of 800rad/min,
Cross-linking reaction is carried out, product is obtained.
The mass ratio of the polypropylene fibre master batch and the modified honeysuckle powder is 85:15；
The additive amount of the organic titanium cross-linking agent Tyzor371 is 0.1% of the modification honeysuckle powder gross mass containing reaction promoter,
The additive amount of the inorganic fire retardants is the 6.5% of polypropylene fibre master batch quality；
The inorganic fire retardants is made of red phosphorus, antimony oxide, zinc borate, acrylic resin, mass ratio 6:1:3:50.
After above-mentioned product is packed into double screw extruder melting extrusion cooling, it is granulated through pelletizer, obtains honeysuckle plant source
Polypropylene fibre master batch.
Wherein, the melting temperature of double screw extruder is 182-245 DEG C, engine speed 900rad/min, feeding revolving speed
For 1000rad/min, the revolving speed of pelletizer is 1100rad/min.
Step 5, spinning (3.2dtex*62mm)
Melt extruded machine temperature is set as 167 °C, by above-mentioned honeysuckle plant source polypropylene fibre master batch through metering pump after temperature is stablized
It is added after metering, continues to be heated to melt completely, molten mass is subjected to melt spinning via spinneret orifice, using leading for the first time
It stretches, second of drawing-off, third time drawing-off, sizing, winding and be formed again, obtain polypropylene fiber；
Wherein, spinneret orifice surface roughness Ra≤0.2 μm, surface static contact angle WCA >=85 °；
First time drawing temperature is 93 DEG C, and second of drawing temperature is 102 DEG C, and third time drawing temperature is 115 DEG C.
1, the honeysuckle plant source polypropylene fibre master batch of embodiment 1-3 is detected, wherein the testing result of main indicator is shown in
Table 1:
Table 1:
2, step 5 spinning is passed through using honeysuckle plant source polypropylene fibre master batch of the examination criteria FZT52003-1993 to embodiment 1-3
3.2dtex*62mm honeysuckle plant source polypropylene fibre master batch fiber product made from step is detected, the wherein detection of main indicator
It the results are shown in Table 2:
Table 2:
Remarks: total burning time uses UL94；Edge-melting smoulder in side when burning has slight candle smell, and flame is small, ashless
Cinder, combustion parts are transparence, non-friable.
3, fiber product (3.2dtex* made of the honeysuckle plant source polypropylene fibre master batch to 1-3 of embodiment of the present invention preparation
After 62mm) washing 50 times and 100 times, indices are measured using examination criteria FZT52003-1993, are shown in Table 3.
Table 3:
4, fiber product (3.2dtex*62mm) made of the honeysuckle plant source polypropylene fibre master batch for preparing 1-3 of the embodiment of the present invention
Longitude and latitude 68D/24F plain cloth is weaved into, 190T is tested using national standard " GB/T 4802.1-1997 ", and measurement is fluffed
Ball effect, is shown in Table 4.
Table 4:
As it can be seen that fabric made by the polypropylene fiber of polypropylene fibre master batch preparation in honeysuckle plant source of the present invention, pilling fluffing resistant performance is good,
Pilling fluffing resistant grade is not less than 4 grades, scared slight pilling, or even slightly scared no pilling.
Plant source polypropylene fibre master batch performance prepared by the present invention is summarized:
(1) by being detected to honeysuckle plant source polypropylene fibre master batch prepared by above-described embodiment 1-3, obtained honeysuckle
Plant source polypropylene fibre master batch, particle is uniform, regular shape, and particle surface is moist, no even grain, no clast, honeysuckle plant source polypropylene fibre
Master batch particle size uniformity is 95.8-99.1%, and oxygen index (OI) (OI) is 29-30；
(2) 3.2dtex*62mm honeysuckle plant source polypropylene fibre master batch made from honeysuckle plant source polypropylene fibre master batch prepared by the present invention
Fiber product, line density deviation ratio are 0.7-1.2%, and length variation rate is 0.01-0.06%, breaking strength 7.9-8.3cN/
Dtex, elongation at break 25.8-30.4%, fault 2.7-2.8mg/100g, the ultimate strength coefficient of variation (CV) 6.5-6.8%,
Excellent fireproof performance, burning time 9.4-8.5s, combustion rating V-1.
(3) 3.2dtex*62mm honeysuckle plant source polypropylene fibre made from honeysuckle plant source polypropylene fibre master batch prepared by the present invention
Master batch fiber product, after repeatedly washing, every mechanical performance is hardly reduced, and after washing 50 times, breaking strength is
7.7-8.4cN/dtex, elongation at break 32.6-35.1%, combustion rating are V-1 grades；After washing 100 times, breaking strength is
6.8-7.6cN/dtex, elongation at break 35.5-38.1%, combustion rating are V-1 grades.
(4) fabric made by the polypropylene fiber of polypropylene fibre master batch preparation in honeysuckle plant source of the present invention, pilling fluffing resistant performance
Good, scared slight pilling, or even slightly scared no pilling, pilling fluffing resistant grade are not less than 4 grades.
By specific data as it can be seen that honeysuckle plant source polypropylene fibre master batch and made fiber product prepared by embodiment 2
The master batch and fibre property highest of preparation are a kind of optimal production and processing methods.
Unless otherwise indicated, percentage employed in the present invention is mass percent, and the ratio is quality
Ratio.Method of the invention is equally applicable to the plant sources such as wormwood, bluish dogbane, folium isatidis, peppermint, motherwort, reaches basic phase
Same technical effect, since length is limited, no longer expansion is repeated one by one herein.
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 plant source polypropylene fibre master batch, it is characterised in that:
The plant source polypropylene fibre master batch is polypropylene fibre master batch and modified honeysuckle powder blended melting preparation；The polypropylene fibre master batch and institute
The mass ratio for stating modified honeysuckle powder is 85:15.
2. a kind of plant source polypropylene fibre master batch according to claim 1, it is characterised in that:
Fiber product made from the plant source polypropylene fibre master batch, line density deviation ratio are 0.7-1.2%, and length variation rate is 0.01-
0.06%, breaking strength 7.9-8.3cN/dtex, elongation at break 25.8-30.4%, fault 2.7-2.8mg/100g, fracture
Strength coefficient of variation 6.5-6.8%, the burning time of flame retardant property are 9.4-8.5s, combustion rating V-1.
3. a kind of preparation method of plant source polypropylene fibre master batch, it is characterised in that: the preparation method includes modified honeysuckle powder
The preparation of preparation and honeysuckle plant source polypropylene fibre master batch.
4. a kind of preparation method of plant source polypropylene fibre master batch according to claim 3, it is characterised in that: the modified gold and silver
Pollen, compatibility is good, and mesh number is 10000 mesh, density 1.08-1.25g/cm3, apparent viscosity 30-50mPa.s, honeysuckle fibre
Dimension cellulose content is 20.7-26.0%.
5. a kind of preparation method of plant source polypropylene fibre master batch according to claim 3, it is characterised in that: the modified gold and silver
The preparation of pollen after mixing 50 parts of honeysuckle powders with the starch of 15-20 parts of chitin and 4-6 part, adjusts pH with sodium carbonate
Afterwards, 50-70 parts of deionized waters are added and are heated to 51-62 DEG C of mixing 30min, is distilled after gains are shaken up, is then dissolved in 40-
In 60 parts of deionized waters, 10-20 parts of acrylic acid of addition are put into close in mixer after semi-permeable membrane constantly washes 0.8-1.6 hours
After refining 1.0-1.6 hours, naturally dry is pulverized, is crushed, and obtains modified honeysuckle powder.
6. a kind of preparation method of plant source polypropylene fibre master batch according to claim 5, it is characterised in that:
After the sodium carbonate is adjusted, pH 7-8；
Using vacuum distillation, distillation time is 0.5-8 hours for the distillation.
7. a kind of preparation method of plant source polypropylene fibre master batch according to claim 3, it is characterised in that:
The method also includes reaction promoter is added, 2.6-3.2% is added into modified honeysuckle powder in the addition reaction promoter
Reaction promoter, be heated up to 40-50 DEG C, stirred with the speed of 900rad/min, is uniformly mixed.
8. a kind of preparation method of plant source polypropylene fibre master batch according to claim 3, it is characterised in that:
The preparation of the honeysuckle plant source polypropylene fibre master batch melts polypropylene fibre master batch, at 198 DEG C with the speed of 800rad/min
4-8min is stirred, the modification honeysuckle powder containing reaction promoter, inorganic fire retardants and organic titanium cross-linking agent Tyzor371 is added, after
The continuous speed with 800rad/min stirs 15min, is granulated, obtains honeysuckle plant source polypropylene fibre master batch.
9. a kind of preparation method of plant source polypropylene fibre master batch according to claim 3, it is characterised in that:
The preparation of the honeysuckle plant source polypropylene fibre master batch, the inorganic fire retardants, by red phosphorus, antimony oxide, zinc borate, third
Olefin(e) acid resin composition, mass ratio 6:1:3:50.
10. a kind of preparation method of plant source polypropylene fibre master batch according to claim 3, it is characterised in that:
The preparation of the honeysuckle plant source polypropylene fibre master batch, the melting temperature of double screw extruder are 182-245 DEG C, pelletizer
Revolving speed is 900-1100rad/min.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811457135.5A CN109503946A (en) | 2018-11-30 | 2018-11-30 | A kind of plant source polypropylene fibre master batch and preparation method thereof |
| CN201911135803.7A CN111253675A (en) | 2018-11-30 | 2019-11-19 | Plant source PP master batch and preparation method and application thereof |
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| CN201811457135.5A CN109503946A (en) | 2018-11-30 | 2018-11-30 | A kind of plant source polypropylene fibre master batch and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253675A (en) * | 2018-11-30 | 2020-06-09 | 中科纺织研究院（青岛）有限公司 | Plant source PP master batch and preparation method and application thereof |
| CN112030263A (en) * | 2020-09-17 | 2020-12-04 | 慈溪金轮复合纤维有限公司 | Polypropylene fiber and preparation process thereof |
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2018
- 2018-11-30 CN CN201811457135.5A patent/CN109503946A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111253675A (en) * | 2018-11-30 | 2020-06-09 | 中科纺织研究院（青岛）有限公司 | Plant source PP master batch and preparation method and application thereof |
| CN112030263A (en) * | 2020-09-17 | 2020-12-04 | 慈溪金轮复合纤维有限公司 | Polypropylene fiber and preparation process thereof |
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Application publication date: 20190322 |