CN106188775A - Organosilane crosslinked polyethylene coating materials that a kind of Radix Notoginseng Flos Lonicerae is compounding and preparation method thereof - Google Patents

Abstract

The present invention discloses the organosilane crosslinked polyethylene coating materials that a kind of Radix Notoginseng Flos Lonicerae is compounding, it is made up of the raw material of following weight portion: Low Density Polyethylene 60 80, vinyltrimethoxy silane 6 12, 2, 5 dimethyl 2, 5 bis(t-butylperoxy) hexanes 0.5 1.5, tealeaf residue 20 30, beta-schardinger dextrin-12 16, citric acid 48, methine sodium phosphate 0.5 2, Radix Notoginseng 46, Flos Lonicerae 59, ethyl acetate 25 35, emulsifying agent T 80 24, phthalic acid two (2 ethyl hexyl) ester 13, accelerant CZ 0.8 1.5, sodium hydroxide solution is appropriate, distilled water is appropriate, Alumen 0.5 1.5.The present invention is carried out inclusion by grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag add in toothpaste sheet film Radix Notoginseng, Flos Lonicerae extract, has safety and medicinal slow release effect, additionally has the feature such as low cost, pollution-free, the splendid feature of environmental protection.

Description

Organosilane crosslinked polyethylene coating materials that a kind of Radix Notoginseng-Flos Lonicerae is compounding and preparation method thereof

Technical field

The invention belongs to technical field of polymer materials, be specifically related to the compounding crosslinked with silicane of a kind of Radix Notoginseng-Flos Lonicerae and gather Ethylene 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.

Sheet material is for the packaging of Flexible tube for toothpaste, and its content lotion of toothpaste is direct and the oral contact of human body.Therefore Whether proper the selection of packaging material is, and direct relation the healthy of people.In the past few years, food-safety problem increasingly causes The attention of people.From tripolycyanamide event several years ago, to plasticiser disturbance in recent years, then to New Zealand's poison milk powder case, nothing Do not affect the nerve that people are fragile to food safety.For toothpaste sheet material, it is also possible to regard " directly contacting human body " as A kind of packaging material, how to ensure that some additives in package stock will not react with the composition in mastic, Cheng Liao Problem faced by firstly the need of.

For toothpaste sheet material, main material or polyethylene and the material such as polypropylene and aluminium foil, the most poly-second The production of alkene material can add the chemical substances such as antioxidant, opening agent, slipping agent, and these materials are in the effect of lotion of toothpaste Under (lotion of toothpaste be well a kind of " extracting substance "), can migrate to mastic from thin film, the change of paste properties may be caused Change.Hao Xihai, Sun Miao et al. embed fourth with beta-schardinger dextrin-in " the clove oil microcapsule antibacterial packing film " literary composition delivered Microcapsule anti-bacterial agent prepared by essential oil, adds to and prepares Antibiotic Membrane in polyvinyl alcohol, and to Microencapsulated Slow anti-microbial property Detecting, polymer carries food preservative functional components, by slowly discharging in food transport and storing process To antiseptic effect.

Summary of the invention

For the deficiencies in the prior art, the invention provides the organosilane crosslinked polyethylene film that a kind of Radix Notoginseng-Flos Lonicerae is compounding Material and preparation method thereof.

The organosilane crosslinked polyethylene coating materials that a kind of Radix Notoginseng-Flos Lonicerae is compounding, is made up of the raw material of following weight portion: low-density Polyethylene 60-80 part, vinyltrimethoxy silane 6-12 part, 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane 0.5-1.5 part, tealeaf residue 20-30 part, beta-schardinger dextrin-12-16 part, citric acid 4-8 part, methine sodium phosphate 0.5-2 part, Radix Notoginseng 4-6 part, Flos Lonicerae 5-9 part, ethyl acetate 25-35 part, emulsifying agent T-80 2-4 part, phthalic acid two (2-ethyl hexyl) ester 1- 3 parts, accelerant CZ 0.8-1.5 part, sodium hydroxide solution is appropriate, and distilled water is appropriate, Alumen 0.5-1.5 part.

Specifically comprise the following steps that

(1) preparation of grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag:

1., by tealeaf residue drying and pulverize, crossing 80-100 mesh sieve, the Folium Camelliae sinensis ground-slag obtained is immersed in sodium hydroxide solution 0.5-2.5 hour, thoroughly wash with the distilled water of 60-70 DEG C afterwards, standby for being dried 18-25 hour in case in 70-90 DEG C；

2., the Folium Camelliae sinensis ground-slag after activation processing is immersed in the ternary being made up of beta-schardinger dextrin-, citric acid, methine sodium phosphate In aqueous solution, after supersound process 10-30 minute, oil bath is heated to 80-110 DEG C and is sufficiently stirred at this temperature, and 2-4 is little in reaction Time, filtering after having reacted, filtering residue is product, is washed at neutrality, 50-70 DEG C be dried 20-25 hour, obtains β-ring and sticks with paste Essence grafting Folium Camelliae sinensis ground-slag；

(2) Radix Notoginseng, the preparation of Flos Lonicerae/Benexate Hydrochloride:

1., powder is dried and be ground into Radix Notoginseng, Flos Lonicerae, add ethyl acetate, hot reflux extraction 1-in the water-bath of 60-80 DEG C 3 hours, filtered while hot, united extraction liquid, add appropriate distilled water after cooling, in mixed liquor, add emulsifying agent T-80, Homogenizing 15-30 minute under the conditions of 5000-8000 rev/min, obtains emulsion；

2., weigh a certain amount of distilled water, add the grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag that step (1) obtains, fully after infiltration, Emulsifying emulsion completely is poured in beta-schardinger dextrin-solution, stirs inclusion 20-30 minute, stand 0.5-1.5 hour After, sucking filtration, wash, be dried, obtain Radix Notoginseng, Flos Lonicerae/Benexate Hydrochloride；

(3) preparation of the polyethylene of Silane Grafted:

Low Density Polyethylene, vinyltrimethoxy silane and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane are mixed Close uniformly, be placed in hermetic container after at least 12 hours, add frit reaction extruding pelletization in double screw extruder, after drying Sealing saves backup；

(4) prepared by Radix Notoginseng, Flos Lonicerae/Benexate Hydrochloride, Low Density Polyethylene and the step (3) step (2) prepared The polyethylene pellet of Silane Grafted puts into mix homogeneously in high-speed mixer, controls rotating speed and is 800-1000 rev/min, 80-130 After DEG C mixing 20-30 minute, add Alumen and surplus stock, continue mixing 30-60 minute, be blended by double screw extruder and squeeze Go out, after water cooled, pelletizing, obtain pellet；

(5) pellet blowfilm shaping on inflation film manufacturing machine that step (4) is obtained.

Wherein, the concentration of described sodium hydroxide solution be mass fraction be 25%-30%.

The present invention compared with prior art has the advantage that

(1) Radix Notoginseng, Flos Lonicerae are additives common in lotion of toothpaste, not only give off a strong fragrance, stable, and have can subside a swelling and stop Bitterly, effect of promoting blood circulation to remove blood stasis, add in polyethylene coating materials base material, can from toothpaste sheet film under the effect of lotion of toothpaste Slowly migrate in mastic, safe to the human body nontoxic, and have certain medicinal efficacy.

(2) additionally the present invention uses grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag that Radix Notoginseng, Flos Lonicerae extract are carried out inclusion, protects Hold the bactericidal antiphlogistic effect of Folium Camelliae sinensis ground-slag, improved the bioavailability of tealeaf residue, additionally Radix Notoginseng, Flos Lonicerae are also had slow release Effect, the polyethylene coating materials of preparation has the feature such as low cost, pollution-free, the splendid feature of environmental protection.

(3) present invention selects Alumen as producing outside water preparation, it is also possible to is uniformly dispersed in matrix as nucleator, is formed Homodisperse network, makes the homogeneous granular of spherocrystal height of generation, forms the spherocrystal granule of tiny densification, changes the chi of spherocrystal Very little, make strand have crystallization rate quickly at relatively high temperatures, the number of the spherocrystal of generation is many, and size is little, and is distributed Uniformly, thus improve mechanical property and the optical property of organosilane crosslinked polyethylene.

Detailed description of the invention

The organosilane crosslinked polyethylene coating materials that Radix Notoginseng-Flos Lonicerae is compounding, is made up of the raw material of following weight portion (kilogram): low close Degree polyethylene 70, vinyltrimethoxy silane 10,2,5-dimethyl-2,5-bis(t-butylperoxy) hexane 1, tealeaf residue 25, beta-schardinger dextrin-15, citric acid 6, methine sodium phosphate 1, Radix Notoginseng 5, Flos Lonicerae 8, ethyl acetate 30, emulsifying agent T-80 3, adjacent Phthalic acid two (2-ethyl hexyl) ester 2, accelerant CZ 1, sodium hydroxide solution is appropriate, and distilled water is appropriate, Alumen 1.

Wherein, the concentration of described sodium hydroxide solution be mass fraction be 30%.

Specifically comprise the following steps that

(1) preparation of grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag:

1., by tealeaf residue drying and pulverize, crossing 100 mesh sieves, it is little that the Folium Camelliae sinensis ground-slag obtained is immersed in sodium hydroxide solution 2 Time, thoroughly wash with the distilled water of 65 DEG C afterwards, standby for being dried 20 hours in case in 80 DEG C；

2., the Folium Camelliae sinensis ground-slag after activation processing is immersed in the ternary being made up of beta-schardinger dextrin-, citric acid, methine sodium phosphate In aqueous solution, supersound process is after 20 minutes, and oil bath is heated to 90 DEG C and is sufficiently stirred at this temperature, reacts 3 hours, has reacted Filtering after one-tenth, filtering residue is product, is washed to neutrality, is dried 22 hours, obtains grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag at 60 DEG C；

(2) Radix Notoginseng, the preparation of Flos Lonicerae/Benexate Hydrochloride:

1., by Radix Notoginseng, Flos Lonicerae drying and be ground into powder, add ethyl acetate, in the water-bath of 70 DEG C, to extract 2 little in hot reflux Time, filtered while hot, united extraction liquid, add appropriate distilled water after cooling, in mixed liquor, add emulsifying agent T-80,7000 Under the conditions of rev/min, homogenizing 20 minutes, obtain emulsion；

2., weigh a certain amount of distilled water, add the grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag that step (1) obtains, fully after infiltration, Emulsifying emulsion completely is poured in beta-schardinger dextrin-solution, stirring inclusion 25 minutes, after standing 1 hour, sucking filtration, water Wash, be dried, obtain Radix Notoginseng, Flos Lonicerae/Benexate Hydrochloride；

(3) preparation of the polyethylene of Silane Grafted:

Low Density Polyethylene, vinyltrimethoxy silane and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane are mixed Close uniformly, be placed in hermetic container after at least 12 hours, add frit reaction extruding pelletization in double screw extruder, after drying Sealing saves backup；

(4) prepared by Radix Notoginseng, Flos Lonicerae/Benexate Hydrochloride, Low Density Polyethylene and the step (3) step (2) prepared The polyethylene pellet of Silane Grafted puts into mix homogeneously in high-speed mixer, and controlling rotating speed is 900 revs/min, 90 DEG C of mixing 25 After minute, add Alumen and surplus stock, continue mixing 40 minutes, by double screw extruder blending extrusion, water cooled, pelletizing After obtain pellet；

(5) pellet blowfilm shaping on inflation film manufacturing machine that step (4) is obtained.

Performance data after tested: hot strength (MPa): MD:97, TD:112；Tension fracture elongation rate (%): MD:196, TD:91；Puncture strength (N): 5.2.

Claims (3)

1. the organosilane crosslinked polyethylene coating materials that Radix Notoginseng-Flos Lonicerae is compounding, it is characterised in that by the raw material group of following weight portion Become: Low Density Polyethylene 60-80 part, vinyltrimethoxy silane 6-12 part, 2,5-dimethyl-2, the double (t-butyl peroxy of 5- Base) hexane 0.5-1.5 part, tealeaf residue 20-30 part, beta-schardinger dextrin-12-16 part, citric acid 4-8 part, methine sodium phosphate 0.5-2 Part, Radix Notoginseng 4-6 part, Flos Lonicerae 5-9 part, ethyl acetate 25-35 part, emulsifying agent T-80 2-4 part, phthalic acid two (2-ethyl Oneself) ester 1-3 part, accelerant CZ 0.8-1.5 part, sodium hydroxide solution is appropriate, and distilled water is appropriate, Alumen 0.5-1.5 part.

2. the preparation method of the organosilane crosslinked polyethylene coating materials compounded according to a kind of Radix Notoginseng-Flos Lonicerae described in claims 1, It is characterized in that, specifically comprise the following steps that

(1) preparation of grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag:

1., by tealeaf residue drying and pulverize, crossing 80-100 mesh sieve, the Folium Camelliae sinensis ground-slag obtained is immersed in sodium hydroxide solution 0.5-2.5 hour, thoroughly wash with the distilled water of 60-70 DEG C afterwards, standby for being dried 18-25 hour in case in 70-90 DEG C；

2., the Folium Camelliae sinensis ground-slag after activation processing is immersed in the ternary being made up of beta-schardinger dextrin-, citric acid, methine sodium phosphate In aqueous solution, after supersound process 10-30 minute, oil bath is heated to 80-110 DEG C and is sufficiently stirred at this temperature, and 2-4 is little in reaction Time, filtering after having reacted, filtering residue is product, is washed at neutrality, 50-70 DEG C be dried 20-25 hour, obtains β-ring and sticks with paste Essence grafting Folium Camelliae sinensis ground-slag；

(2) Radix Notoginseng, the preparation of Flos Lonicerae/Benexate Hydrochloride:

1., powder is dried and be ground into Radix Notoginseng, Flos Lonicerae, add ethyl acetate, hot reflux extraction 1-in the water-bath of 60-80 DEG C 3 hours, filtered while hot, united extraction liquid, add appropriate distilled water after cooling, in mixed liquor, add emulsifying agent T-80, Homogenizing 15-30 minute under the conditions of 5000-8000 rev/min, obtains emulsion；

2., weigh a certain amount of distilled water, add the grafted by beta cyclodextrin Folium Camelliae sinensis ground-slag that step (1) obtains, fully after infiltration, Emulsifying emulsion completely is poured in beta-schardinger dextrin-solution, stirs inclusion 20-30 minute, stand 0.5-1.5 hour After, sucking filtration, wash, be dried, obtain Radix Notoginseng, Flos Lonicerae/Benexate Hydrochloride；

(3) preparation of the polyethylene of Silane Grafted:

Low Density Polyethylene, vinyltrimethoxy silane and 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane are mixed Close uniformly, be placed in hermetic container after at least 12 hours, add frit reaction extruding pelletization in double screw extruder, after drying Sealing saves backup；

(4) prepared by Radix Notoginseng, Flos Lonicerae/Benexate Hydrochloride, Low Density Polyethylene and the step (3) step (2) prepared The polyethylene pellet of Silane Grafted puts into mix homogeneously in high-speed mixer, controls rotating speed and is 800-1000 rev/min, 80-130 After DEG C mixing 20-30 minute, add Alumen and surplus stock, continue mixing 30-60 minute, be blended by double screw extruder and squeeze Go out, after water cooled, pelletizing, obtain pellet；

(5) pellet blowfilm shaping on inflation film manufacturing machine that step (4) is obtained.

3. the preparation side of the organosilane crosslinked polyethylene coating materials compounded according to a kind of Radix Notoginseng-Flos Lonicerae described in claims 1,2 Method, it is characterised in that the concentration of described sodium hydroxide solution be mass fraction be 25%-30%.