CN107652507A - A kind of preparation method of fire-retardant plastic sheeting - Google Patents
A kind of preparation method of fire-retardant plastic sheeting Download PDFInfo
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- CN107652507A CN107652507A CN201710896623.5A CN201710896623A CN107652507A CN 107652507 A CN107652507 A CN 107652507A CN 201710896623 A CN201710896623 A CN 201710896623A CN 107652507 A CN107652507 A CN 107652507A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2323/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
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Abstract
The invention belongs to plastics arts, specially a kind of preparation method of fire-retardant plastic sheeting, concretely comprise the following steps：(1) modified flame-retardant agent is prepared；(2) plastic sheeting is prepared：A, basic grain is made；B, slurry is adjusted；C, will be stirred 10 15 minutes in magnetic stirring apparatus after basic grain, slurry, 38 parts of acrylate fiber, 5 15 parts of mixing of 15 20 parts of calcium oxide, 10 20 parts of modified flame-retardant agent, 20 35 parts of 15 part, nanometer sodium bentonite of polyvinyl alcohol, coupling agent that activity degree is 500 600mL, then using plastic film blowing machine extrusion blown film, you can obtain plastic sheeting.This method is simple and easy, and this method is simple and easy, and the product produced has more excellent tensile strength, elongation at break, light transmittance, water resistance, antibacterial ability compared with prior art.
Description
【Technical field】
The present invention relates to plastics arts, and in particular to a kind of preparation method of fire-retardant plastic sheeting.
【Background technology】
Plastic products majority has inflammability, and this brings many hidden danger to its product using safety.As plastics exist
The extensive use of building, furniture, traffic, Aeronautics and Astronautics, electrical equipment etc., improving flame retardant of plastic, oneself turns into very urgent
Problem.
Chinese patent CN201510216597.8 discloses a kind of flame retardant plastics, the plastics by following portions by weight material
It is made:Plastics 40-50 parts, filler 15-25 parts, melamine cyanurate 10-20 parts, antimony trioxide 5-10 parts, APP 5-
10 parts, polybutylene terephthalate vinegar 10-20 parts, composite flame-retardant agent 15-30 parts, iron oxide 10-20 parts, auxiliary agent 5-10 parts.
But the patent plastic production cost is high, density is big, use it is very heavy, be not suitable for large-scale popularization as standard multi-purpose resistance
Film is fired to use.
Chinese patent CN201310561438.2 discloses a kind of PP/HDPE flame-retardant alloys plastics, by following weight parts group
It is grouped into：50 parts of polypropylene, high density polyethylene (HDPE) 20-40 parts, ethylene propylene diene rubber 10-30 parts, fire retardant 15-25 parts are described
Fire retardant is made up of the poly- loop coil phosphoric acid vinegar diamides of 40-60wt% and 40-60wt% melamine cyanurates.But the invention is special
The flame-retardant alloy plastics that profit provides prepare difficulty, and preparation cost is high, are not suitable for promoting.
In order to solve, existing flame retardant plastics film preparation cost is high, product quality is not high, fire-retardant coefficient is not high, antibacterial ability
The problem of not strong, now provide it is a kind of prepare it is simple, prepare that cost is low, flame retardant plastics film of good product quality.
【The content of the invention】
The goal of the invention of the present invention is：For it is above-mentioned the problem of, the present invention provides a kind of system of fire-retardant plastic sheeting
Preparation Method, this method is simple and easy, and the product produced has more excellent tensile strength, fracture compared with prior art
Elongation, light transmittance, water resistance, antibacterial ability.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of preparation method of fire-retardant plastic sheeting, specifically includes following steps：
(1) modified flame-retardant agent is prepared：According to percent by weight, xylenylphosphate 5-10%, melamine 5- are weighed
10%th, antimony oxide 5-10%, expansile graphite 5-15%, red phosphorus 15-25%, chlorinated paraffin 18-30%, magnesium hydroxide
After 15-30% mixing, dispersion mixing 0.1-1 hours are carried out using ultrasonic wave, are then irradiated 1-2 hours using gamma-rays,
Progress anaerobic heating in heater is then placed in, is divided into three phases, the first stage is warming up to 3-5 points of 100 degrees Centigrade
Clock, second stage were warming up to for 300 degrees Centigrade 1-3 minutes, and the phase III is warming up to 500 degrees Celsius of addition 20-30 seconds, then
Vacuumize and naturally cool to normal temperature after being cooled to 100 degrees Celsius, obtain mixed powder, by mixed powder and medical grade white oil according to
Weight ratio is 100:Mortar grinder is carried out after 1-2 mixing, crosses 1000 mesh sieves, then carries out being dried in vacuo 0.5-1.5 hours, you can
Modified flame-retardant agent is obtained, it is standby；
(2) plastic sheeting is prepared：
A, in parts by weight, by list after low density polyethylene (LDPE) 50-100 parts, Chinese cassia tree extract powder 5-20 parts being mixed
Screw rod or double-screw plastic extrusion machine extruding pelletization obtain basic grain, standby；
B, by terephthalate 1-5 parts, glycerine 2-6 parts, urea 1-5 parts, water 25-35 parts, barium sulfate 5-10 parts, cunning
Stone flour 8-10 parts Mixed adjustment is slurry, standby；
C, by basic grain, slurry, acrylate fiber 3-8 parts, activity degree be 500-600mL calcium oxide 15-20 parts,
In magnetic after modified flame-retardant agent 10-20 parts, polyvinyl alcohol 1-5 parts, nanometer sodium bentonite 20-35 parts, the mixing of coupling agent 5-15 parts
10-15 minutes are stirred in power agitator, blown film are then extruded using plastic film blowing machine, you can obtain plastic sheeting.
Further illustrate, in step (1), the parameter of ultrasonic wave is 1000-1200 hertz.
Further illustrate, in step (2), the Chinese cassia tree extract powder is prepared by following methods：
The cinnamon bark of 100-150 parts by weight is weighed, then crushed 10-50 mesh sieves, is then carried out by high-temperature steam
Modified ground cinnamon is obtained after thermal cracking, is subsequently added into the ethanol solution that mass fraction is 85%, carries out husky formula extraction 30-40
Minute, obtain extract solution, then carry out distill 3-4 hours obtain distillate, then by mass concentration be 1-3% diethyl ether solution
Distillate is extracted, separates and merges ether extraction liquid, then reclaim ether, is sprayed after surplus solution is concentrated dry
It is dry to obtain Chinese cassia tree extract powder.
Further illustrate, microwave radiation exaraction is also carried out during husky formula extraction；The power of the microwave is 500-600W.
Further illustrate, mass concentration is 1-3% diethyl ether solution：The volume ratio of distillate is 1:3-6.
Further illustrate, the coupling agent is titanate coupling agent DL171, titanate coupling agent KH550, and titanate esters are coupled
It is one or more in agent DL602, titanate coupling agent KH560, titanate coupling agent KH570.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
First：Chinese cassia tree extract powder is also added in the plastic sheeting of the application, there can be good antibacterial ability, it is low close
Degree polyethylene forms hydrogen bond with Chinese cassia tree extract powder or covalent bond improves, and improves the tensile strength of plastic sheeting, fracture is stretched
Long rate；And a certain proportion of barium sulfate, talcum powder are with the addition of between raw material, raw material is scattered during interaction improves blown film
Property and mobility, the support of additional fire retardant further increase the dispersiveness and mobility of raw material during blown film so that product
Shaping has beneficial stability；It is not only have dispersiveness with mobility it is ensured that being blow molded into during quantity film is prepared
The stability of type, the applicant has found by research, with the addition of a certain proportion of terephthalate 1-5 parts, glycerine 2-6
Part, urea 1-5 parts, water 25-35 parts so that raw material has excellent bridging property and plasticization so that during blow molding
By the calcium oxide of organic phase, nanometer sodium bentonite, acrylate fiber, valence link is broken after being plastified, being crosslinked, uniformly edge
Between macromolecule, the casting films of network structure are formed, improve translucency, the tensile strength of plastic sheeting, additional addition gathers
Vinyl alcohol collective effect after the very high calcium oxide of activation grade has good network structure with nanometer sodium bentonite can improve
The water resistance of plastic sheeting.
Second：Fire retardant in the application is by xylenylphosphate 5-10%, melamine 5-10%, antimony oxide 5-
10%th, by this after expansile graphite 5-15%, red phosphorus 15-25%, chlorinated paraffin 18-30%, magnesium hydroxide 15-30% mixing
The modified obtained modified flame-retardant agent of the technological means of application has more preferable dispersiveness, mechanical performance, heat endurance and fire-retardant
Property, this makes it possible to add less fire retardant when making plastic sheeting can also play good fire resistance, in order to up to
The modified flame-retardant agent for accounting for raw material 1 15 to percent 20 is with the addition of to more excellent flame retardant effect；Modified flame-retardant agent
In xylenylphosphate with good fire resistance, C-P chemical bonds with good water resistance, but it is to evaporate
Strong, the poor heat resistance of property；Chlorinated paraffin has good compression strength, lubricity, anti-irradiation, anti-oxidant and fire resistance, still
Its poor heat resistance；It is low to add melamine hygroscopicity, will not separate out, alternative part resin, reduces adhesive dosage, has
But when its progress fire retardant effect, addition is big, and dispersiveness is poor；Red phosphorus and high polymer material intermiscibility are poor；Di(2-ethylhexyl)phosphate
Toluene ester, chlorinated paraffin, melamine mix the chemical bond rupture for carrying out heating latter three, mutually fusion so that mixture has
There is an effect learnt from other's strong points to offset one's weaknesses, the red phosphorus of addition, antimony oxide, magnesium hydroxide can enter one as retardant synergist to fire retardant
Step is modified, and is introduced magnesium ion, antimony ion, phosphonium ion and has been haveed the function that collaboration, and modification is irradiated after ultrasonic disperse
The sign property for changing material part can be played, then again in the process of lapping of white oil so that mixed material is further crosslinked, fully
Molecule face identical fire retardant is obtained, so as to improve the polymolecularity of modified flame-retardant agent compound, the high-compatibility of base material and resistance
Fuel efficiency fruit so that fire retardant can improve not only with flame retardant effect also with lubrication peptizaiton during plastic sheeting is made
The mobility of melt, it ensure that the stability of blow molding.
To sum up for 2 points, plastic sheeting that the application is prepared is in anti-flammability, tensile strength, elongation at break, thoroughly
Light rate, water resistance, there is excellent effect on antibacterial ability.
3rd, the materials of the application are simple, abundance, cheap；Its preparation technology simplifies, is feasible, operation side
Just, production easy to spread.
【Embodiment】
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Embodiment is closed, the present invention is expanded on further.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention,
It is not intended to limit the present invention.
Embodiment 1：
A kind of preparation method of fire-retardant plastic sheeting, specifically includes following steps：
(1) modified flame-retardant agent is prepared：According to percent by weight, xylenylphosphate 5%, melamine 5%, three are weighed
After aoxidizing two antimony 5%, expansile graphite 5%, red phosphorus 20%, chlorinated paraffin 30%, the mixing of magnesium hydroxide 30%, 1000 hertz are used
Ultrasonic wave hereby carries out dispersion mixing 0.1 hour, is then irradiated 1 hour using gamma-rays, is then placed in heater
Row anaerobic heats, and is divided into three phases, the first stage is warming up to 100 degrees Centigrade 3 minutes, and second stage is warming up to 300
Degrees Centigrade 1 minute, phase III are warming up to 500 degrees Celsius and added 20 seconds, then vacuumize after being cooled to 100 degrees Celsius certainly
Normal temperature so is cooled to, obtains mixed powder, according to weight ratio is 100 by mixed powder and medical grade white oil:Ground after 1 mixing
Alms bowl is ground, and crosses 1000 mesh sieves, then carries out vacuum drying 0.5 hour, you can modified flame-retardant agent is obtained, it is standby；
(2) plastic sheeting is prepared：
A, in parts by weight, by twin-screw plastics after 50 parts of low density polyethylene (LDPE), 5 parts of Chinese cassia tree extract powder being mixed
Extruder extruding pelletization obtains basic grain, standby；
B, by 8 parts of 1 part of terephthalate, 2 parts of glycerine, 1 part of urea, 25 parts of water, 5 parts of barium sulfate, talcum powder mixing
Slurry is adjusted to, it is standby；
C, by basic grain, slurry, 3 parts of acrylate fiber, 15 parts of calcium oxide, the modified flame-retardant that activity degree is 500mL
10 parts of agent, 20 parts of 1 part, nanometer sodium bentonite of polyvinyl alcohol, 3 parts of titanate coupling agent DL171, titanate coupling agent
KH5503 parts, 3 parts of titanate coupling agent DL602,3 parts of titanate coupling agent KH560,3 parts of titanate coupling agent KH570 are mixed
Stirred after conjunction in magnetic stirring apparatus 10 minutes, blown film is then extruded using plastic film blowing machine, you can obtain plastic sheeting.
Wherein, Chinese cassia tree extract powder is prepared by following methods：The cinnamon bark of 100 parts by weight is weighed, then powder
The broken mesh sieve of mistake 10, modified ground cinnamon then is obtained after high-temperature steam carries out thermal cracking, being subsequently added into mass fraction is
85% ethanol solution, carry out husky formula and extract 30 minutes, and extract solution is obtained using 500W microwave radiation exaractions, then steamed
Evaporate 3 hours and obtain distillate, then according to diethyl ether solution：The volume ratio of distillate is 1:The ether that 3 mass concentration is 1% is molten
Liquid extracts to distillate, separates and merges ether extraction liquid, then reclaim ether, is sprayed after surplus solution is concentrated
It is dried to obtain Chinese cassia tree extract powder.
Embodiment 2：
A kind of preparation method of fire-retardant plastic sheeting, specifically includes following steps：
(1) modified flame-retardant agent is prepared：According to percent by weight, weigh xylenylphosphate 10%, melamine 10%,
After antimony oxide 10%, expansile graphite 15%, red phosphorus 22%, chlorinated paraffin 18%, magnesium hydroxide 15% mix, use
1200 hertz of ultrasonic wave carries out dispersion mixing 1 hour, is then irradiated 2 hours using gamma-rays, is then placed in heater
Middle progress anaerobic heating, is divided into three phases, the first stage is warming up to 100 degrees Centigrade 5 minutes, and second stage is warming up to
300 degrees Centigrades 3 minutes, phase III are warming up to 500 degrees Celsius and added 30 seconds, then vacuumize and be cooled to 100 degrees Celsius
After naturally cool to normal temperature, obtain mixed powder, according to weight ratio be 100 by mixed powder and medical grade white oil:2 mixing are laggard
Row mortar grinder, 1000 mesh sieves are crossed, then carry out vacuum drying 1.5 hours, you can modified flame-retardant agent is obtained, it is standby；
(2) plastic sheeting is prepared：
A, in parts by weight, will be moulded after 20 parts of 100 parts of low density polyethylene (LDPE), Chinese cassia tree extract powder mixing by single screw rod
Material extruder extruding pelletization obtains basic grain, standby；
B, it is 5 parts of terephthalate, 6 parts of glycerine, 5 parts of urea, 35 parts of water, 10 parts of barium sulfate, 10 parts of talcum powder is mixed
Conjunction is adjusted to slurry, standby；
C, by basic grain, slurry, 8 parts of acrylate fiber, 20 parts of calcium oxide, the modified flame-retardant that activity degree is 600mL
In magnetic agitation after 5 parts of 20 parts of agent, 35 parts of 5 part, nanometer sodium bentonite of polyvinyl alcohol, titanate coupling agent KH570 kinds mixing
Stirred in device 15 minutes, blown film is then extruded using plastic film blowing machine, you can obtain plastic sheeting.
Wherein, Chinese cassia tree extract powder is prepared by following methods：The cinnamon bark of 150 parts by weight is weighed, then powder
The broken mesh sieve of mistake 50, modified ground cinnamon then is obtained after high-temperature steam carries out thermal cracking, being subsequently added into mass fraction is
85% ethanol solution, carry out husky formula and extract 40 minutes, and extract solution is obtained using 600W microwave radiation exaractions, then steamed
Evaporate 4 hours and obtain distillate, then according to diethyl ether solution：The volume ratio of distillate is 1:The ether that 6 mass concentration is 3% is molten
Liquid extracts to distillate, separates and merges ether extraction liquid, then reclaim ether, is sprayed after surplus solution is concentrated
It is dried to obtain Chinese cassia tree extract powder.
Embodiment 3：
A kind of preparation method of fire-retardant plastic sheeting, specifically includes following steps：
(1) modified flame-retardant agent is prepared：According to percent by weight, xylenylphosphate 7%, melamine 8%, three are weighed
After aoxidizing two antimony 9%, expansile graphite 10%, red phosphorus 15%, chlorinated paraffin 25%, the mixing of magnesium hydroxide 26%, 1050 are used
The ultrasonic wave of hertz carries out dispersion mixing 0.2 hour, is then irradiated 1.2 hours using gamma-rays, is then placed in heater
Middle progress anaerobic heating, is divided into three phases, the first stage is warming up to 100 degrees Centigrade 4 minutes, and second stage is warming up to
300 degrees Centigrades 2 minutes, phase III are warming up to 500 degrees Celsius and added 22 seconds, then vacuumize and be cooled to 100 degrees Celsius
After naturally cool to normal temperature, obtain mixed powder, according to weight ratio be 100 by mixed powder and medical grade white oil:1 mixing is laggard
Row mortar grinder, 1000 mesh sieves are crossed, then carry out vacuum drying 0.8 hour, you can modified flame-retardant agent is obtained, it is standby；
(2) plastic sheeting is prepared：
A, in parts by weight, by single screw rod or double after 60 parts of low density polyethylene (LDPE), 8 parts of Chinese cassia tree extract powder being mixed
Screw rod plastic extruder extruding pelletization obtains basic grain, standby；
B, by 9 parts of 2 parts of terephthalate, 3 parts of glycerine, 2 parts of urea, 26 parts of water, 6 parts of barium sulfate, talcum powder mixing
Slurry is adjusted to, it is standby；
C, by basic grain, slurry, 4 parts of acrylate fiber, 16 parts of calcium oxide, the modified flame-retardant that activity degree is 520mL
12 parts of agent, 22 parts of 2 part, nanometer sodium bentonite of polyvinyl alcohol, 4 parts of titanate coupling agent KH550, titanate coupling agent KH560
2 parts, stirred 12 minutes in magnetic stirring apparatus after 2 parts of titanate coupling agent KH570 mixing, then squeezed using plastic film blowing machine
Go out blown film, you can obtain plastic sheeting.
Wherein, Chinese cassia tree extract powder is prepared by following methods：The cinnamon bark of 120 parts by weight is weighed, then powder
The broken mesh sieve of mistake 20, modified ground cinnamon then is obtained after high-temperature steam carries out thermal cracking, being subsequently added into mass fraction is
85% ethanol solution, carry out husky formula and extract 32 minutes, and extract solution is obtained using 520W microwave radiation exaractions, then steamed
Evaporate 3.2 hours and obtain distillate, then according to diethyl ether solution：The volume ratio of distillate is 1:4 mass concentration is 2.5% second
Ethereal solution extracts to distillate, separates and merges ether extraction liquid, ether is then reclaimed, after surplus solution is concentrated
Spray drying obtains Chinese cassia tree extract powder.
Embodiment 4：
A kind of preparation method of fire-retardant plastic sheeting, specifically includes following steps：
(1) modified flame-retardant agent is prepared：According to percent by weight, xylenylphosphate 8%, melamine 6%, three are weighed
After aoxidizing two antimony 7%, expansile graphite 8%, red phosphorus 25%, chlorinated paraffin 22%, the mixing of magnesium hydroxide 24%, 1100 hertz are used
Ultrasonic wave hereby carries out dispersion mixing 0.5 hour, is then irradiated 1.5 hours, is then placed in heater using gamma-rays
Anaerobic heating is carried out, is divided into three phases, the first stage is warming up to 100 degrees Centigrade 3.5 minutes, and second stage is warming up to
300 degrees Centigrades 1.5 minutes, phase III are warming up to 500 degrees Celsius and added 25 seconds, then vacuumize that to be cooled to 100 Celsius
Normal temperature is naturally cooled to after degree, obtains mixed powder, according to weight ratio is 100 by mixed powder and medical grade white oil:After 2 mixing
Mortar grinder is carried out, crosses 1000 mesh sieves, then carries out vacuum drying 1.0 hours, you can modified flame-retardant agent is obtained, it is standby；
(2) plastic sheeting is prepared：
A, in parts by weight, by after 70 parts of low density polyethylene (LDPE), the mixing of 12 parts of Chinese cassia tree extract powder by single screw rod or
Double-screw plastic extrusion machine extruding pelletization obtains basic grain, standby；
B, it is 3 parts of terephthalate, 4 parts of glycerine, 3 parts of urea, 30 parts of water, barium sulfate 5-10 parts, 9 parts of talcum powder is mixed
Conjunction is adjusted to slurry, standby；
C, by basic grain, slurry, 5 parts of acrylate fiber, 17 parts of calcium oxide, the modified flame-retardant that activity degree is 550mL
15 parts of agent, 29 parts of 3 part, nanometer sodium bentonite of polyvinyl alcohol, 4 parts of titanate coupling agent DL171, titanate coupling agent
Stirred after the mixing of DL6025 parts in magnetic stirring apparatus 13 minutes, blown film is then extruded using plastic film blowing machine, you can moulded
Expect film.
Wherein, Chinese cassia tree extract powder is prepared by following methods：The cinnamon bark of 130 parts by weight is weighed, then powder
The broken mesh sieve of mistake 40, modified ground cinnamon then is obtained after high-temperature steam carries out thermal cracking, being subsequently added into mass fraction is
85% ethanol solution, carry out husky formula and extract 35 minutes, and extract solution is obtained using 540W microwave radiation exaractions, then steamed
Evaporate 3.2 hours and obtain distillate, then according to diethyl ether solution：The volume ratio of distillate is 1:5 mass concentration is 1.5% second
Ethereal solution extracts to distillate, separates and merges ether extraction liquid, ether is then reclaimed, after surplus solution is concentrated
Spray drying obtains Chinese cassia tree extract powder.
Embodiment 5：
A kind of preparation method of fire-retardant plastic sheeting, specifically includes following steps：
(1) modified flame-retardant agent is prepared：According to percent by weight, xylenylphosphate 6%, melamine 6%, three are weighed
After aoxidizing two antimony 6%, expansile graphite 12%, red phosphorus 18%, chlorinated paraffin 28%, the mixing of magnesium hydroxide 24%, 1150 are used
The ultrasonic wave of hertz carries out dispersion mixing 0.8 hour, is then irradiated 1.8 hours using gamma-rays, is then placed in heater
Middle progress anaerobic heating, is divided into three phases, and the first stage is warming up to 100 degrees Centigrade 4.5 minutes, second stage heating
To 300 degrees Centigrade 2.5 minutes, the phase III was warming up to 500 degrees Celsius and added 28 seconds, then vacuumizes and is cooled to 100 and takes the photograph
Normal temperature is naturally cooled to after family name's degree, obtains mixed powder, according to weight ratio is 100 by mixed powder and medical grade white oil:1 mixing
After carry out mortar grinder, cross 1000 mesh sieves, then carry out vacuum drying 1.2 hours, you can obtain modified flame-retardant agent, it is standby；
(2) plastic sheeting is prepared：
A, in parts by weight, will be moulded after 18 parts of 90 parts of low density polyethylene (LDPE), Chinese cassia tree extract powder mixing by twin-screw
Material extruder extruding pelletization obtains basic grain, standby；
B, by 8 parts of 4 parts of terephthalate, 5 parts of glycerine, 4 parts of urea, 32 parts of water, 8 parts of barium sulfate, talcum powder mixing
Slurry is adjusted to, it is standby；
C, by basic grain, slurry, 7 parts of acrylate fiber, 19 parts of calcium oxide, the modified flame-retardant that activity degree is 580mL
In magnetic agitation after 12 parts of 18 parts of agent, 32 parts of 4 part, nanometer sodium bentonite of polyvinyl alcohol, titanate coupling agent KH550 mixing
Stirred in device 14 minutes, blown film is then extruded using plastic film blowing machine, you can obtain plastic sheeting.
Wherein, Chinese cassia tree extract powder is prepared by following methods：The cinnamon bark of 140 parts by weight is weighed, then powder
The broken mesh sieve of mistake 45, modified ground cinnamon then is obtained after high-temperature steam carries out thermal cracking, being subsequently added into mass fraction is
85% ethanol solution, carry out husky formula and extract 38 minutes, and extract solution is obtained using 585W microwave radiation exaractions, then steamed
Evaporating 3-4 hours obtains distillate, then according to diethyl ether solution：The volume ratio of distillate is 1:5 mass concentration is 2% ether
Solution extracts to distillate, separates and merges ether extraction liquid, then reclaim ether, is sprayed after surplus solution is concentrated
Mist is dried to obtain Chinese cassia tree extract powder.
Comparative example 1：
The plastic sheeting of purchase on the market.
Comparative example 2：
Essentially identical with the preparation method of embodiment 5, difference is：Do not carry out preparing modified flame-retardant agent step, and using general
Aglow phosphorus is substituted.
Comparative example 3：
Essentially identical with the preparation method of embodiment 5, difference is：It is not added with Chinese cassia tree extract powder.
Following detection is carried out to embodiment 1-5 and comparative example 1-3 plastic sheeting
The mechanical property of film：
According to national standard《Stretched plastic film method for testing performance》(GB/13022-1991), with sampling cutter produce 15mm ×
120mm rectangle samples, are put into 23 DEG C of temperature, flat 12h in the climatic chamber of relative humidity 50%, with smart electronicses pull test
Machine determines the tensile strength and elongation at break of edible film, and specimen length is 80mm, test speed 200mm/ between two chucks
Min, each sample determine 3 times.
Light transmittance：Plastic sheeting is sliced into 5cm × 3cm sizes, is attached to the side of cuvette, is placed in ultraviolet-visible point
Its light transmittance is surveyed in light photometer at 660nm wavelength, each sample determines 3 times.
Rate of perviousness：According to national standard《Packaging material test method-rate of perviousness》(GB/T16928-1997), tested with penetrability
Instrument determines, and each sample determines 3 times.
OTR oxygen transmission rate：According to national standard《Plastic sheeting and thin slice gas-premeable test method-pressure differential method》(GB/
T1038-2000), determined with gas-premeable tester, each sample determines 3 times.
The bacteriostatic test of film：Suppress the bacteriostasis property of method measure composite membrane using disk.With micropipette by 0.1mL bacterium
The Escherichia coli bacteria suspension that concentration is 105CFU/mL imports nutrient agar, and coating is uniform, aeration-drying 10min, will be multiple
The sequin that diameter about 6mm is made in film is closed, plating medium center is placed in, 24h and 48h is cultivated at 37 DEG C, observes and surveys
Measure bacteriostatic diameter.Each sample does 3 groups of parallel tests.Not add the composite membrane of cinnamic acid as blank control.
Fire resistance：The flammable test method of plastics and standard (UL94 flammability tests).
Testing result contrast table
As seen from the above table, by embodiment 1-5 compared with comparative example 1, tensile strength improves at least 5MPa, fracture is stretched
Long rate improves at least 20%, light transmittance and at least reduces 12%, it was demonstrated that the technical scheme of the application can be blow molded into
By the calcium oxide of organic phase, nanometer sodium bentonite, acrylate fiber, valence link breaks after being plastified, being crosslinked during type
Split, be uniformly embedded between macromolecule, form the casting films of network structure, improve translucency, the tensile strength of plastic sheeting；Implement
1-5 is compared with comparative example 1 for example, and vapor transmission coefficient reduces at least 0.3 10-13[g/ (cmsPa), oxygen pass through
Rate reduces at least 0.75 10-5[cm3/(m2DPa)] demonstrate, polyvinyl alcohol is in the very high calcium oxide of activation grade with receiving
There is rice sodium bentonite collective effect after good network structure can improve the water resistance of plastic sheeting；Pass through embodiment 1-
5 compared with comparative example 1, and inhibition zone is far longer than comparative example 1, it was demonstrated that plastic sheeting prepared by the application has excellent antibacterial
Effect；Embodiment 5 is not added with reducing 2.59MP, extension at break in the tensile strength of Chinese cassia tree extract powder compared with comparative example 3
Rate improves at least 17%, antibacterial ability also without so good.Embodiment 5 is not added with modified flame-retardant agent compared with comparative example 2
The technical characteristic fire resistance compared to the application compared to more excellent.Prepared in summary using the preparation method of the application
Plastic sheeting on tensile strength, elongation at break, light transmittance, water resistance, antibacterial ability homogeneously than comparative example 1 have more
Add excellent performance.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore limitation of the scope of the invention can not be interpreted as.It should be pointed out that for the person of ordinary skill of the art,
Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection model of the present invention
Enclose.Therefore, protection scope of the present invention should be determined by the appended claims.
Claims (8)
- A kind of 1. preparation method of fire-retardant plastic sheeting, it is characterised in that：Specifically include following steps：(1) modified flame-retardant agent is prepared：According to percent by weight, weigh xylenylphosphate 5-10%, melamine 5-10%, Antimony oxide 5-10%, expansile graphite 5-15%, red phosphorus 15-25%, chlorinated paraffin 18-30%, magnesium hydroxide 15-30% After mixing, dispersion mixing 0.1-1 hours are carried out using ultrasonic wave, then 1-2 hours is irradiated using gamma-rays, is then placed in Anaerobic heating is carried out in heater, is divided into three phases, the first stage is warming up to 100 degrees Centigrade 3-5 minutes, second-order Section was warming up to for 300 degrees Centigrade 1-3 minutes, and the phase III is warming up to 500 degrees Celsius of addition 20-30 seconds, then vacuumized cold But to normal temperature is naturally cooled to after 100 degrees Celsius, mixed powder is obtained, is according to weight ratio with medical grade white oil by mixed powder 100:Mortar grinder is carried out after 1-2 mixing, crosses 1000 mesh sieves, then carries out being dried in vacuo 0.5-1.5 hours, you can be modified Fire retardant, it is standby；(2) plastic sheeting is prepared：A, in parts by weight, by single screw rod after low density polyethylene (LDPE) 50-100 parts, Chinese cassia tree extract powder 5-20 parts being mixed It is standby or double-screw plastic extrusion machine extruding pelletization obtains basic grain；B, by terephthalate 1-5 parts, glycerine 2-6 parts, urea 1-5 parts, water 25-35 parts, barium sulfate 5-10 parts, talcum powder 8-10 parts Mixed adjustment is slurry, standby；C, it is 500-600mL calcium oxide 15-20 parts, modification by basic grain, slurry, acrylate fiber 3-8 parts, activity degree Stirred after fire retardant 10-20 parts, polyvinyl alcohol 1-5 parts, nanometer sodium bentonite 20-35 parts, the mixing of coupling agent 5-15 parts in magnetic force Stirring 10-15 minutes in device are mixed, blown film are then extruded using plastic film blowing machine, you can obtain plastic sheeting.
- A kind of 2. preparation method of fire-retardant plastic sheeting according to claim 1, it is characterised in that：In step (1), The parameter of ultrasonic wave is 1000-1200 hertz.
- A kind of 3. preparation method of fire-retardant plastic sheeting according to claim 1, it is characterised in that：In step (2), The Chinese cassia tree extract powder is prepared by following methods：The cinnamon bark of 100-150 parts by weight is weighed, then crushed 10-50 mesh sieves, then carries out hot tearing by high-temperature steam Modified ground cinnamon is obtained after solution, is subsequently added into the ethanol solution that mass fraction is 85%, carries out husky 30-40 points of formula extraction Clock, obtain extract solution, then carry out distill 3-4 hours obtain distillate, then by mass concentration be 1-3% diethyl ether solution pair Distillate is extracted, and is separated and is merged ether extraction liquid, then reclaim ether, is spray-dried after surplus solution is concentrated Obtain Chinese cassia tree extract powder.
- A kind of 4. preparation method of fire-retardant plastic sheeting according to claim 3, it is characterised in that：During husky formula extraction Also carry out microwave radiation exaraction；The power of the microwave is 500-600W.
- A kind of 5. preparation method of fire-retardant plastic sheeting according to claim 3, it is characterised in that：Mass concentration is 1- 3% diethyl ether solution：The volume ratio of distillate is 1:3-6.
- A kind of 6. preparation method of fire-retardant plastic sheeting according to claim 1, it is characterised in that：The coupling agent is Titanate coupling agent DL171, titanate coupling agent KH550, titanate coupling agent DL602, titanate coupling agent KH560, metatitanic acid It is one or more in ester coupling agent KH570.
- A kind of 7. preparation method of fire-retardant plastic sheeting according to claim 1, it is characterised in that：The talcum powder Spend for 5 μm -10 μm.
- A kind of 8. preparation method of fire-retardant plastic sheeting according to claim 1, it is characterised in that：The nanometer sodium base Swelling soil granularity is 500nm-1000nm.
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| CN111286142A (en) * | 2020-03-09 | 2020-06-16 | 福建省睿星纺织科技有限公司 | Flame-retardant packaging plastic film and preparation method thereof |
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| CN112250385A (en) * | 2020-10-23 | 2021-01-22 | 舒城诚鑫建材有限公司 | Light flame-retardant heat-insulating material for building exterior wall and preparation method thereof |
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