CN106046523A - Modified graphene-polyethylene film material for toothpaste sheeting and preparation method thereof - Google Patents
Modified graphene-polyethylene film material for toothpaste sheeting and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a modified graphene-polyethylene film material for toothpaste sheeting, made from the following materials according to parts by weight: 60-70 parts of linear low-density polyethylene, 8-15 parts of waxy corn starch, 8-15 parts of plant fiber powder, 3-6 parts of a silane coupling agent, 25-35 parts of degradable calcium carbonate master batch, 10-18 parts of vinyl-terminated silicone oil, 0.3-0.8 part of hydrogen-containing silicone oil, suitable sulfuric acid solution, suitable platinum catalyst, 2-5 parts of 7-hydroxy-4-methylcoumarin, 1.5-3 parts of graphene oxide, 0.5-1.5 parts of vitamin C, suitable 30% ammonia solution and suitable deionized water. After using, the polyethylene film material of the invention can be degraded into water and carbon dioxide under natural conditions within 6-18 months, the biodegradation speed is high, no white pollution is caused, and the requirement for environmental protection is met; in addition, composite film prepared by adding the modified graphene is uniform in dispersion and stable in performance.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of toothpaste sheet material modified graphene-polyethylene
Coating materials and preparation method thereof.
Background technology
What dentifrice tube packaging was currently mainly used is multiple tube packaging, and the feature of a highly significant of composite soft tube is
Its body material is composite sheet, and composite sheet is that the coating materials produced by multiple different materials by the way of compound is multiple
It is combined.Its production technology is flexible, as can also be combined by extrusion with dry type is compound, can be combined in flakes after printing
Material tubulation, it is also possible to carrying out printing tubulation after producing into sheet material;Draw materials extensively, can be polyolefin, polyamides for material
Amine, polyester, aluminium foil, paper etc., can be blown film, casting films, co-extrusion film, biaxial stretching film, vacuum for the type of coating materials
Aluminizer, coated film etc..This makes composite sheet all have the highest at aspects such as barrier property, physical and mechanical properties, outward appearances
Motility.
At present, composite sheet packaging material market being used on toothpaste are mainly plastic-aluminum combined sheet material (ABL) and overall plastic
Composite sheet (PBL), this two classes composite sheet almost occupies whole toothpaste packing market.
The problem of most popular plastic-aluminum sheet material maximum is exactly to be difficult to be recycled after it uses.Aluminium foil is multiple with plastics
Simple approach delamination cannot be passed through, although occurred much reclaiming way after conjunction, but mostly in order to separate aluminium foil and plastics
Acid, alkali or organic solvent can be used, the most costly, and environment is produced secondary pollution.And environmental protection composite sheet packaging
Material, because it has low cost, reclaiming pollution-free, easy, the feature such as degradable, will become the master of following environment-friendly package material
Stream.
Wang Mingsheng, Sun Heng have delivered advantage and application one literary composition of an environmental protection composite hose sheet material, describe composite soft tube
Present situation and the development trend of environmental protection flexible pipe, just add the environment-friendlythin thin film of pearl filler in mechanical property, deflection, environmental protection, fall
The aspects such as solution are analyzed and have been discussed.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of toothpaste sheet material modified graphene-polyethylene coating materials and
Its preparation method, the problem solving polyethylene coating materials environment-friendly degradable, ensure again meet the mechanical property of dimerization product and use requirement.
A kind of toothpaste sheet material modified graphene-polyethylene coating materials, is made up of the raw material of following weight portion: linea low density
Polyethylene 60-70 part, wax corn starch 8-15 part, Plant fiber's powder 8-15 part, silane coupler 3-6 part, degradation-type carbon
Acid calcium master batch 25-35 part, vinyl-terminated silicone oil 10-18 part, containing hydrogen silicone oil 0.3-0.8 part, sulfuric acid solution is appropriate, platinum catalyst
In right amount, Hymecromone 2-5 part, graphene oxide 1.5-3 part, vitamin C 0.5-1.5 part, the ammonia of 30% is molten
Liquid is appropriate, and deionized water is appropriate;
Described environment-friendly degradable type calcium carbonate master batch is composed of the following raw materials by weight: Low Density Polyethylene 10-30 part, n-octyl
Ferrocene 10-15 part, polylactic acid 0.2-0.5 part, Tissuemat E 1-2 part, titanate coupling agent 0.5-2.5 part, nano-calcium carbonate
25-35 part, paraffin oil is appropriate.
Specifically comprise the following steps that
(1) preparation of degradation-type calcium carbonate master batch:
1. high speed mixing smelting machine high-speed rotation, then the titanate coupling agent diluted by paraffin oil, spray are put into, in advance by nano-calcium carbonate
Entering in calcium carbonate material, heat up discharging after stirring 10-30 minute, obtains surface-treated calcium carbonate after drying;
2., with through surface-treated calcium carbonate for master batch core, same to Low Density Polyethylene, octyl ferrocene, polylactic acid, poly-
Ethylene waxes puts in homogenizer, and it is blended uniform in 60-100 DEG C to control temperature, after mix homogeneously, puts into mixed on low speed
Machine combination cooling, is subsequently adding double screw extruder extruding pelletization as environment-friendly degradable type calcium carbonate master batch;
(2) preparation of organosilicone elastic microsphere:
1., wax corn starch is joined in sulfuric acid solution, in the thermostatical oil bath of 35-45 DEG C, with 100-200 rev/min
After the speed of clock stirs 5-7 days, product is centrifuged repeatedly and is washed to neutrality, be vacuum dried to obtain nanometer starch crystal solid powder
End;
2., nanometer starch crystal pressed powder, Plant fiber's powder are added in deionized water, ultrasonic disperse 3-10 minute, then will
Pour in the aqueous dispersions of nanometer starch crystal after vinyl-terminated silicone oil and containing hydrogen silicone oil mix homogeneously, 8000-on homogenizer
Under the conditions of 12000 revs/min, homogenizing 3-15 minute, adds platinum catalyst, is the most under agitation warmed up to 40-60 DEG C of reaction 1-
3 hours, after reaction terminates, being performing centrifugal separation on, the organosilicone elastic that vacuum drying obtains nanometer starch crystal-Plant fiber's coating is micro-
Ball;
(3) preparation of modified graphene:
First by graphene oxide disperse in deionized water, at normal temperatures ultrasonic vibration stir 5-8 hour, add 7-hydroxyl-
4-methylcoumarin, stirs 3-5 hour at 30-50 DEG C, and the ammonia spirit regulation pH value being subsequently adding 30% stirs 2-to 9-10
4 hours, add vitamin C and react at 70-90 DEG C and within 15-20 hour, obtain modified mixed liquor, by this modification mixed liquor sucking filtration
Obtain solid matter, then be washed with deionized to neutrality, be dried under vacuum to constant weight in 40-70 DEG C, i.e. obtain modified graphene;
(4) elastic microsphere step (2) obtained adds in the high-speed mixer that rotating speed is 800-1000 rev/min, adds silicon
Alkane coupling agent is mixed with uniformly, is subsequently adding linear low density polyethylene, modified graphene that step (3) obtains, controls temperature
Degree is blended uniformly within 60-100 DEG C, after mix homogeneously, puts into low speed mixer combination cooling, is subsequently adding twin-screw extrusion
Machine extruding pelletization;
(5) calcium carbonate master batch step (1) obtained obtains plastic pellet with step (4) and mixs homogeneously in high-speed mixer,
Then through steps such as pellet conveying, fusion plastification, extrusion, inflation, corona, rollings on film blowing device, a kind of tooth-paste sheet is prepared
Material modified graphene-polyethylene coating materials.
Described platinum catalyst is the aqueous isopropanol of chloroplatinic acid, and its content is for accounting for vinyl-terminated silicone oil and hydrogeneous with Pt
The 4-6ppm of silicon oil mixture total amount.
The present invention compared with prior art has the advantage that
(1) the polyethylene coating materials that the present invention is prepared by adding environment-friendly degradable type calcium carbonate master batch is after using, it is possible at 6-
Being decomposed into water and carbon dioxide in 18 months under field conditions (factors), biodegradation rate is fast, without producing white pollution, meets
The requirement of environmental protection.
(2) present invention utilizes nanometer starch crystal, Plant fiber's powder emulsifying vinyl-terminated silicone oil and containing hydrogen silicone oil, passes through
Si-H addition reaction prepares organosilicone elastic microsphere.This organosilicone elastic microsphere surface is adsorbed with that degradable starch is nanocrystalline and plant
Fiber powder, has the mobility of excellence, dispersibility, has toughness and the intensity of excellence simultaneously, improves the deflection of coating materials.
(3) modifying agent that the present invention chooses is Hymecromone, and its molecule contains hydroxyl, ester group and conjugation
Structures etc., can interact with oxy radical generation hydrogen bond and the-key etc. such as the carbonyl in graphene oxide and carboxyl, pass through
The modified graphene reduced by vitamin C and obtain, is conducive to the dispersibility improving and improving Graphene in polyethylene, strengthens
Interface binding power, can regulate the quality of polyethylene hot property etc., prepare by controlling the addition of modified graphene
Laminated film is uniformly dispersed, stable performance.
Detailed description of the invention
A kind of toothpaste sheet material modified graphene-polyethylene coating materials, is made up of the raw material of following weight portion (kilogram): linear
Low Density Polyethylene 70, wax corn starch 10, Plant fiber's powder 10, silane coupler 4, degradation-type calcium carbonate master batch 30,
Vinyl-terminated silicone oil 15 parts, containing hydrogen silicone oil 0.5 part, sulfuric acid solution is appropriate, and platinum catalyst is appropriate, 7-hydroxy-4-methyl tonkabean
Element 3, graphene oxide 2, vitamin C 1, the ammonia spirit of 30% is appropriate, and deionized water is appropriate;
Described environment-friendly degradable type calcium carbonate master batch is composed of the following raw materials by weight: Low Density Polyethylene 25 parts, n-octyl two
Cyclopentadienyl ferrum 12 parts, polylactic acid 0.4 part, Tissuemat E 1 part, titanate coupling agent 1.5 parts, nano-calcium carbonate 30 parts, paraffin oil is appropriate.
Described platinum catalyst is the aqueous isopropanol of chloroplatinic acid, and its content is for accounting for vinyl-terminated silicone oil and hydrogeneous with Pt
The 5ppm of silicon oil mixture total amount.
Specifically comprise the following steps that
(1) preparation of degradation-type calcium carbonate master batch:
1. high speed mixing smelting machine high-speed rotation, then the titanate coupling agent diluted by paraffin oil, spray are put into, in advance by nano-calcium carbonate
Entering in calcium carbonate material, heat up discharging after stirring 20 minutes, obtains surface-treated calcium carbonate after drying;
2., with through surface-treated calcium carbonate for master batch core, same to Low Density Polyethylene, octyl ferrocene, polylactic acid, poly-
Ethylene waxes puts in homogenizer, and it is blended uniform in 80 DEG C to control temperature, after mix homogeneously, puts into low speed mixer and mixes
Close cooling, be subsequently adding double screw extruder extruding pelletization as environment-friendly degradable type calcium carbonate master batch;
(2) preparation of organosilicone elastic microsphere:
1., wax corn starch is joined in sulfuric acid solution, in the thermostatical oil bath of 40 DEG C, with the speed of 150 revs/min
After stirring 6 days, product is centrifuged repeatedly and is washed to neutrality, be vacuum dried to obtain nanometer starch crystal pressed powder;
2., nanometer starch crystal pressed powder, Plant fiber's powder are added in deionized water, ultrasonic disperse 8 minutes, then by ethylene
Pour into after base end-blocking silicone oil and containing hydrogen silicone oil mix homogeneously in the aqueous dispersions of nanometer starch crystal, on homogenizer 10000 revs/min
Under the conditions of clock, homogenizing 10 minutes, add platinum catalyst, are the most under agitation warmed up to 50 DEG C and react 2 hours, after reaction terminates,
Being performing centrifugal separation on, vacuum drying obtains the organosilicone elastic microsphere of nanometer starch crystal-Plant fiber's coating;
(3) preparation of modified graphene:
First by graphene oxide disperse in deionized water, at normal temperatures ultrasonic vibration stir 5-8 hour, add 7-hydroxyl-
4-methylcoumarin, stirs 3-5 hour at 30-50 DEG C, and the ammonia spirit regulation pH value being subsequently adding 30% stirs 2-to 9-10
4 hours, add vitamin C and react at 70-90 DEG C and within 15-20 hour, obtain modified mixed liquor, by this modification mixed liquor sucking filtration
Obtain solid matter, then be washed with deionized to neutrality, be dried under vacuum to constant weight in 40-70 DEG C, i.e. obtain modified graphene;
(4) elastic microsphere step (2) obtained adds in the high-speed mixer that rotating speed is 1000 revs/min, adds silane even
Connection agent is mixed with uniformly, is subsequently adding linear low density polyethylene, modified graphene that step (3) obtains, and control temperature exists
It is blended uniformly within 70 DEG C, after mix homogeneously, puts into low speed mixer combination cooling, be subsequently adding double screw extruder extrusion and make
Grain;
(5) calcium carbonate master batch step (1) obtained obtains plastic pellet with step (4) and mixs homogeneously in high-speed mixer,
Then through steps such as pellet conveying, fusion plastification, extrusion, inflation, corona, rollings on film blowing device, a kind of tooth-paste sheet is prepared
Material modified graphene-polyethylene coating materials.
Data after tested: hot strength (MPa): horizontal 22, longitudinal 26;Elongation at break (MPa): horizontal 850, longitudinally
825;Deflection (N): horizontal 3.3, longitudinal 4.2.
Claims (3)
1. toothpaste sheet material modified graphene-polyethylene coating materials, it is characterised in that be made up of the raw material of following weight portion:
Linear low density polyethylene 60-70 part, wax corn starch 8-15 part, Plant fiber's powder 8-15 part, silane coupler 3-6
Part, degradation-type calcium carbonate master batch 25-35 part, vinyl-terminated silicone oil 10-18 part, containing hydrogen silicone oil 0.3-0.8 part, sulfuric acid solution is fitted
Amount, platinum catalyst is appropriate, Hymecromone 2-5 part, graphene oxide 1.5-3 part, vitamin C 0.5-1.5 part,
The ammonia spirit of 30% is appropriate, and deionized water is appropriate;
Described environment-friendly degradable type calcium carbonate master batch is composed of the following raw materials by weight: Low Density Polyethylene 10-30 part, n-octyl
Ferrocene 10-15 part, polylactic acid 0.2-0.5 part, Tissuemat E 1-2 part, titanate coupling agent 0.5-2.5 part, nano-calcium carbonate
25-35 part, paraffin oil is appropriate.
2., according to the preparation method of a kind of toothpaste sheet material modified graphene-polyethylene coating materials described in claims 1, it is special
Levy and be, specifically comprise the following steps that
(1) preparation of degradation-type calcium carbonate master batch:
1. high speed mixing smelting machine high-speed rotation, then the titanate coupling agent diluted by paraffin oil, spray are put into, in advance by nano-calcium carbonate
Entering in calcium carbonate material, heat up discharging after stirring 10-30 minute, obtains surface-treated calcium carbonate after drying;
2., with through surface-treated calcium carbonate for master batch core, same to Low Density Polyethylene, octyl ferrocene, polylactic acid, poly-
Ethylene waxes puts in homogenizer, and it is blended uniform in 60-100 DEG C to control temperature, after mix homogeneously, puts into mixed on low speed
Machine combination cooling, is subsequently adding double screw extruder extruding pelletization as environment-friendly degradable type calcium carbonate master batch;
(2) preparation of organosilicone elastic microsphere:
1., wax corn starch is joined in sulfuric acid solution, in the thermostatical oil bath of 35-45 DEG C, with 100-200 rev/min
After the speed of clock stirs 5-7 days, product is centrifuged repeatedly and is washed to neutrality, be vacuum dried to obtain nanometer starch crystal solid powder
End;
2., nanometer starch crystal pressed powder, Plant fiber's powder are added in deionized water, ultrasonic disperse 3-10 minute, then will
Pour in the aqueous dispersions of nanometer starch crystal after vinyl-terminated silicone oil and containing hydrogen silicone oil mix homogeneously, 8000-on homogenizer
Under the conditions of 12000 revs/min, homogenizing 3-15 minute, adds platinum catalyst, is the most under agitation warmed up to 40-60 DEG C of reaction 1-
3 hours, after reaction terminates, being performing centrifugal separation on, the organosilicone elastic that vacuum drying obtains nanometer starch crystal-Plant fiber's coating is micro-
Ball;
(3) preparation of modified graphene:
First by graphene oxide disperse in deionized water, at normal temperatures ultrasonic vibration stir 5-8 hour, add 7-hydroxyl-
4-methylcoumarin, stirs 3-5 hour at 30-50 DEG C, and the ammonia spirit regulation pH value being subsequently adding 30% stirs 2-to 9-10
4 hours, add vitamin C and react at 70-90 DEG C and within 15-20 hour, obtain modified mixed liquor, by this modification mixed liquor sucking filtration
Obtain solid matter, then be washed with deionized to neutrality, be dried under vacuum to constant weight in 40-70 DEG C, i.e. obtain modified graphene;
(4) elastic microsphere step (2) obtained adds in the high-speed mixer that rotating speed is 800-1000 rev/min, adds silicon
Alkane coupling agent is mixed with uniformly, is subsequently adding linear low density polyethylene, modified graphene that step (3) obtains, controls temperature
Degree is blended uniformly within 60-100 DEG C, after mix homogeneously, puts into low speed mixer combination cooling, is subsequently adding twin-screw extrusion
Machine extruding pelletization;
(5) calcium carbonate master batch step (1) obtained obtains plastic pellet with step (4) and mixs homogeneously in high-speed mixer,
Then through steps such as pellet conveying, fusion plastification, extrusion, inflation, corona, rollings on film blowing device, a kind of tooth-paste sheet is prepared
Material modified graphene-polyethylene coating materials.
3. according to the preparation method of a kind of toothpaste sheet material modified graphene-polyethylene coating materials described in claims 1,2, its
Being characterised by, platinum catalyst is the aqueous isopropanol of chloroplatinic acid, and its content is for account for vinyl-terminated silicone oil and containing hydrogen silicone oil with Pt
The 4-6ppm of amount of the mixture.
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CN106810739A (en) * | 2016-12-02 | 2017-06-09 | 长兴天晟能源科技有限公司 | A kind of functional agglomerate for improving polyethylene packaging film toughness |
CN110684263A (en) * | 2019-10-15 | 2020-01-14 | 福建船政交通职业学院 | Degradable film material and preparation method thereof |
CN112341696A (en) * | 2020-12-16 | 2021-02-09 | 瀚寅(苏州)新材料科技有限公司 | Nano-modified high-barrier membrane and preparation method thereof |
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