CN106832424A - A kind of method that cellulose powder and Biodegradable resin blending modified material prepare inflation film - Google Patents

A kind of method that cellulose powder and Biodegradable resin blending modified material prepare inflation film Download PDF

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Publication number
CN106832424A
CN106832424A CN201710152373.4A CN201710152373A CN106832424A CN 106832424 A CN106832424 A CN 106832424A CN 201710152373 A CN201710152373 A CN 201710152373A CN 106832424 A CN106832424 A CN 106832424A
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cellulose
biodegradable resin
powder
consumption
temperature
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宗敬东
徐荣斌
毛光辉
曹玺
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Suzhou Puli New Material Co Ltd
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Suzhou Puli New Material Co Ltd
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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
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/02—Cellulose; Modified cellulose
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/002—Methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7461—Combinations of dissimilar mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/80—Component parts, details or accessories; Auxiliary operations
    • B29B7/88—Adding charges, i.e. additives
    • B29B7/90—Fillers or reinforcements, e.g. fibres
    • B29B7/92—Wood chips or wood fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/12—Making granules characterised by structure or composition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/16—Auxiliary treatment of granules
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
    • B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/48—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft with intermeshing devices, e.g. screws
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • 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
    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02—Cellulose; Modified cellulose
    • 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
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
    • 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
    • C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/06—Biodegradable
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/16—Applications used for films
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

Abstract

The present invention relates to a kind of blown film technique, and in particular to a kind of method that cellulose powder and Biodegradable resin blending modified material prepare inflation film.The present invention is with biological materials such as timber, stalk, husk, cotton, paper as raw material, crushed through constant temperature, low temperature refining, dry and Biodegradable resin, compatilizer, lubricant, plasticizer and inorganic filler are mixed and compatibility is processed, then carry out mixing granulator, blown film and obtain product.The present invention uses the production technology of unique physics environmental protection, prepares ultra-microfibers element powder and is blended with Biodegradable resin, and dispersion is more uniform, and the film strength and aesthetics of raising open the new method that cellulose is applied in film-like materials.

Description

A kind of cellulose powder and Biodegradable resin blending modified material prepare inflation film Method
Technical field
The present invention relates to a kind of blown film technique, and in particular to change to a kind of cellulose powder and Biodegradable resin blending The method that property material prepares inflation film.
Background technology
Human being's production, a large amount of dependence fossil resources of life are big to being given off in air during using fossil resource The carbon dioxide of amount, makes global warming, causes global extreme climate to change, and causes greatly to lose to the mankind and naturally. Chinese Government promises to undertake in the global climate conference of Paris, to the year two thousand thirty per GDP CO2 emission decline 60-65%, arrives The year two thousand fifty reduces and relies on 50% to petroleum chemicals.
Biomass resource is opened up, new material is extracted and prepared using biomass, reduced carbon emission, develop a circular economy One effective way.From the point of view of the cereal crops of daily mankind plantation, the ratio general 1 of grain and stalk：1, in the market Multiplex starch biolobic material and Biodegradable resin blending (such as CN102373858A), although so there is the concept of biomass, But starch is used, the situation that grain is striven with the mankind is formd, the substantial amounts of foodstuff waste for resulting in.
The present invention utilizes cellulose, the hemicellulose of biomass straw material extraction, by after normal temperature and low temperature refining, becoming As a class novel thin film class materials'use after particle into particle diameter less than 50 microns, and Biodegradable resin blending, thus Open the new route that a new bio material prepares biodegradable intermingling material.
The content of the invention
The purpose of the present invention is to overcome the biomass film in the prior art to need starch, and starch and Biodegradable resin system Standby film elongation at break rate poor performance, the present invention provides a kind of cellulose powder and prepared by Biodegradable resin blending modified material The method of inflation film.
The technical solution adopted in the present invention is as follows：
A kind of method that cellulose powder and Biodegradable resin blending modified material prepare inflation film, including following step Suddenly：
1) cellulose refinement：First by the one-level constant temperature milling equipment that temperature is 10 DEG C -15 DEG C, cellulose is refined to The mesh of particle diameter 100 (i.e. particle diameter is less than 150 μm) below, crush by the micronization for entering back into the two grade low-temp constant temperature that temperature is -10 DEG C Machine, miniaturization obtains micronization cellulose powder；
2) dry：By micronization cellulose powder in high-speed mixer high speed combination drying, moisture content is removed, obtain cellulose Powder；The dry temperature is 100-130 DEG C, dries to water content and is less than 0.2%；
3) mixing and compatibility treatment：Step 2) dried cellulose powder and Biodegradable resin mixing, and add phase Hold agent, lubricant and plasticizer, inorganic filler to be together well mixed and heat, to Biodegradable resin fusing；Mixed melting is equal It is discharged in container after even, mixed material of lowering the temperature to obtain；The heating-up temperature is 130-150 DEG C；
4) mixing granulator：By step 3 after cooling) mixed material, through dual-screw-stem machine extruding pelletization, obtains high content cellulose Masterbatch pellet；Twin-screw extrusion temperature is 120-150 DEG C；
5) blown film：By step 4) obtained in high content cellulose masterbatch pellet be well mixed with Biodegradable resin, directly By twin-screw heating further mixing after extruding blown film or be well mixed using inflation film manufacturing machine, extruding pelletization, then using single spiral shell Bar inflation film manufacturing machine blown film；
Inflation film manufacturing machine of the present invention is more than 30 using draw ratio:1st, spout band forces cooling, spout barrel design band longitudinal direction The single screw rod inflation film manufacturing machine of groove, film blowing machine screw band barrier mixing section and pin mixing refining head are strengthened plastifying with further.Blown film temperature Spend depending on the Biodegradable resin and equipment according to used by.
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 1) described in cellulose be the biologies such as timber, stalk, husk, cotton, paper Material, is preferred from stalk, husk or paper；
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 1) particle diameter of the micronization cellulose powder is less than 50 μm；
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 3) described in Biodegradable resin be degradable aliphatic polyester, such as PBAT (polytetramethylene glycol adipic acid terephthalate), PCL (polycaprolactone), PBS (PBGS), PBSA (polybutadienes Alcohol succinic acid adipate ester), PBST (polytetramethylene glycol succinic acid terephthalate), PLA (PLA) Polymer material One or more materials；
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 3) described in compatilizer be selected from and cellulose, Biodegradable resin have good phase Capacitive, can promote the compatibility of cellulose and Biodegradable resin, step 3 with hydrogen bond and chemical bond) described in compatilizer consumption It is the 1-20% of cellulose powder consumption, preferably to 1-5%；
Described compatilizer is selected from glycerin monostearate, OPE, maleic anhydride grafted polyethylene wax, tristearin The double oleamides of sour acid amides, oleamide, ethylene, erucyl amide, maleic anhydride grafting paraffin, the biological drop of maleic anhydride grafting Solution resin etc.；
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 3) described in lubricant be selected from stearic acid, zinc stearate, calcium stearate, poly- second Alkene wax, OPE, paraffin, oxidized paraffin wax, maleic anhydride grafting paraffin, maleic anhydride grafted polyethylene wax etc., step 3) lubricant quantity described in is the 0.5-5%, preferably 0.5-2% of cellulose powder consumption.
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 3) described in plasticizer be selected from the low mass molecule alcohol chemical combination such as glycerine, D-sorbite Thing, step 3) plasticizer consumption for cellulose powder consumption 0.5-5%, preferably 0.5-2%.
The system of micronization cellulose powder of the present invention and Biodegradable resin blending modified material and inflation film Preparation Method, its further technical scheme is, step 3) described in inorganic filler be talcum powder, calcium carbonate etc., the use of inorganic filler Amount is 0.5 with the ratio of cellulose powder consumption：(5~10), the grain diameter of inorganic filler is less than 50 μm；
Term " biodegradation " of the present invention refers to that organic compound is by microorganism in the presence of microorganism and enzyme Be decomposed into carbon dioxide and water or methane with enzyme, and its contained substance mineralising salt and new biomass.Unless otherwise specified, The usage amount and its ratio of all materials of the present invention are by weight.
Relative to prior art, the present invention has advantages below：
1) the invention provides it is a kind of can with scale, industrialization, low cost using biomass fiber material new way Footpath, especially as stalk, the shell of cereal this class discarded object；Current Biodegradable resin and many selections of biological material blending Starch is biomass, there is a problem of striving grain with people, and starch is the hygroscopic material of a class, makes the shelf-life of intermingling material Have a greatly reduced quality, and cellulose has not facile hydrolysis, the characteristics of the holding time is long；
2) during production estimation, the ratio general 1 of grain and stalk, husk produced by crops:1, sometimes Stalk, husk ratio it is slightly more, prepare new material using the cellulose of the extractions such as stalk, husk, hemicellulose, make These discarded resources are fully utilized, and are beneficial to natural environment, reduce the use to petroleum chemicals, reduce carbon emission；
3) cellulose is due to its special structure so that such material during by industrial application, mostly useization Method, produces very big pressure to environmental protection in process of production, also improves the application cost of this kind of material；The present invention Using physical crushing, the method for the replaceable operation chain chemistry of mixing, this technical problem is solved；
4) present invention prepares ultra-microfibers element powder and and Biodegradable resin using the production technology of unique physics environmental protection Blending, dispersion is more uniform, and the film strength and aesthetics of raising open the new side that cellulose is applied in film-like materials Method.
Specific embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to specific embodiment, to this Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Physical and mechanical properties establishing criteria：GB/T21661-2008 plastic shopping bags.
Embodiment 1
It is first by one-level constant temperature (temperature is 10-15 DEG C) milling equipment, paper fibre element is first thin by discarded paper Change to 100 mesh (150 μm) below, the micronization pulverizer (temperature is set as subzero 10 DEG C) for entering back into two grade low-temp constant temperature is micro- Refinement, particle diameter is less than 15 μm.
Paper powder 20kg that miniaturization particle diameter is 15 μm is added and heat in high mixer combination drying, 120 DEG C of drying temperature, 1 hour or so time, mix to without steam, it is desirable to dry to moisture below 0.2%；
Above-mentioned dried powder 6kg is taken, and PBAT 3kg add high-speed mixer mixed at high speed, add oxidic polyethylene Wax 1kg, 0.03kg zinc stearate and plasticizer glycerine 0.10kg, add the talcum powder 300g that fineness is 2000 mesh, mixed melting Uniformly, heating-up temperature is 135 DEG C, and in mixed process, the powder that will must be bonded in mixer wall was scraped off every 20 minutes.Mixing It is discharged in container after good, is lowered the temperature.
The material that will be mixed is added in double screw extruder, 120-150 DEG C of setting twin-screw extrusion temperature, extrudes pelletizing. The fine powder content of paper is about 57%.
Weigh particle 8kg and the PBAT 7kg that the above is made dry-mixed uniform, make the fine powder content of mixture paper about 30%, Inflation film manufacturing machine extruder blown film, extruder temperature is directly used to be set as 120-150 DEG C, extruder rotating speed 20r/min, hauling speed 15m/min, the film of blowing thickness 0.020mm, and test intensity.
Embodiment 2
High-speed mixer will be added according to case study on implementation 1 made dry miniaturization paper powder 6kg and PBS3kg, and added It is 2000 mesh talcum powder to enter maleic anhydride grafting paraffin 1.2kg and 0.3kg zinc stearate, plasticizer glycerine 0.10kg, fineness 500g, 135 DEG C of heating-up temperature, mixed melting is uniform, in mixed process, must will be bonded at the powder in mixer wall every 20 minutes Scrape off.Cooling in container is discharged to after mixing,
The material that will be mixed is added in double screw extruder, 120-150 DEG C of setting twin-screw extrusion temperature, extrudes pelletizing. Miniaturization paper content of powder is about 54%.
Above-mentioned high-content super-fine paper powder masterbatch 6kg and PBAT (MFR≤5) 10kg is taken, is well mixed.Paper powder Content is 20%.The material that will be mixed further is kneaded by twin-screw heating, extruding pelletization, then is blown using single screw rod inflation film manufacturing machine Film, extruder temperature is set as 120-150 DEG C, and extruder rotating speed 18r/min, hauling speed 15m/min blow thickness The film of 0.020mm, and test intensity.
Embodiment 3
Straw ash dust earth is cleaned out, it is long to be switched to about 5-10mm, dried more than 2 hours for 100 DEG C in baking oven, taken out Dry in the air cool standby.
By the stalk of above-mentioned drying first by one-level constant temperature (temperature is less than 10-15 DEG C) milling equipment, first it is refined to Below, the micronization pulverizer (temperature is set as subzero 10 DEG C) for entering back into two grade low-temp constant temperature is fine for 100 mesh (150 μm) Change, particle diameter is less than 15 μm.
In the equipment for first adding vacuum drying to mix stalk powder 6kg, 100 DEG C of heating-up temperature, heating removes moisture, about Need 1 hour, plus PBSA3kg, glycerin monostearate 0.06kg and 0.2kg stearic acid, talcum powder 200g, plasticizer sorbitol 100g, heating-up temperature is that 145 DEG C of mixed meltings are uniform.Cooling in container is discharged to after mixing.The material that will be mixed adds double In screw extruder, 100-120 DEG C of setting double screw extruder temperature extrudes pelletizing, is made the masterbatch of concentration about 63%.
Take above-mentioned masterbatch 5kg and add PBAT10kg, straw biomass content is 20%.Well mixed extrusion blown film, extrusion Machine temperature is set as 100-120 DEG C, and extruder rotating speed 20r/min, hauling speed 21m/min, blowing thickness 0.020mm's is thin Film, and test intensity.
Embodiment 4
Powdered rice hulls are removed into dust, is dried 2 hours in 100 DEG C of baking oven；Then 100 mesh (150 are crushed at normal temperatures μm) below, the micronization pulverizer (temperature is set as subzero 10-15 DEG C) of cryogenic thermostat being entered back into, miniaturization is small to particle diameter In 15 μm.
The powdered rice hulls that will have been refined are added in vacuum drying mixing apparatus, and 100 DEG C of heating-up temperature, heating removes moisture, about Need 1 hour, take dried powdered rice hulls 6kg and add PCL3kg, Tissuemat E 0.3kg, the stearic acid of maleic anhydride grafting 0.1kg, glycerine 0.1kg, talcum powder 0.4kg, mixed melting are uniform, 150 DEG C of heating-up temperature.
Cooling in container is discharged to after mixed, adds double-screw extruding pelletizing, extrusion temperature to be set as 80-100 DEG C, obtain The masterbatch of the fine powder content 61% of rice husk.
Taking above-mentioned masterbatch 6kg adds 6kgPCL directly to mix, and is extruded after the content 30% of powdered rice hulls micro mist is well mixed and blown Film, 80-100 DEG C of blown film temperature, extruder rotating speed 18r/min, hauling speed 25m/min, the film of blowing thickness 0.015mm is simultaneously Test intensity.
According to preparation method of the invention, the biological material such as timber, stalk, husk, cotton, paper is replaced using starch Material, prepares the film of different content of starch and tests intensity.
Embodiment of the present invention 1-4 and its utilization starch replace the biological materials such as timber, stalk, husk, cotton, paper, Prepare its intensity of the film of different content of starch and elongation at break result is as described in Table 1：
The result of table 1 is tested
As shown by data cellulose blending PBAT is compared with the film tensile strength of starch blending modified PBAT, and the former intensity will Height, but elongation at break compares, it is cellulose modified with more preferable balance, this be due to both dispersion mechanisms, formula not Caused by.The multiplex glycerine gelatinized starch of blown film of starch PBAT blendings in the market, improves dispersiveness, and increase in general Modeling, causes the decline of intensity, and glycerine easily to separate out.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from of the invention In the case of spirit and scope, embodiments of the present invention can be made with various changes, replace and change.

Claims (7)

1. a kind of method that cellulose powder and Biodegradable resin blending modified material prepare inflation film, comprises the following steps：
1) cellulose refinement：First by the one-level constant temperature milling equipment that temperature is 10 DEG C -15 DEG C, cellulose is refined to particle diameter Below 100 mesh, the micronization pulverizer of the two grade low-temp constant temperature that temperature is -10 DEG C is entered back into, miniaturization obtains ultra tiny chemical fibre The plain powder of dimension；The particle diameter of the micronization cellulose powder is less than 50 μm；
2) dry：By micronization cellulose powder in high-speed mixer high speed combination drying, moisture content is removed, dry to moisture content and contain Amount is less than 0.2%, obtains cellulose powder；The dry temperature is 100-130 DEG C；
3) mixing and compatibility treatment：Step 2) dried cellulose powder and Biodegradable resin mixing, and add compatilizer, Lubricant, plasticizer and inorganic filler are together well mixed and heat, to Biodegradable resin fusing；Put after mixed melting is uniform In material to container, mixed material of lowering the temperature to obtain；The heating-up temperature is 130-150 DEG C；Cellulose in the mixed material that cooling is obtained Powder weight content is 50%-75%, balance of Biodegradable resin, compatilizer, lubricant, plasticizer and inorganic filler；
4) mixing granulator：By step 3 after cooling) mixed material, through dual-screw-stem machine extruding pelletization, obtains high content cellulose masterbatch Particle；Twin-screw extrusion temperature is 120-150 DEG C；
5) blown film：By step 4) obtained in high content cellulose masterbatch pellet be well mixed with Biodegradable resin, directly use Inflation film manufacturing machine is extruded blown film or is further kneaded by twin-screw heating, extruding pelletization, then using single screw rod inflation film manufacturing machine blown film.
2. method according to claim 1, it is characterised in that：Step 1) described in cellulose for timber, stalk, husk, Cotton or paper.
3. method according to claim 1, it is characterised in that：Step 3) described in Biodegradable resin be degradable fat Fat adoption ester, the degradable aliphatic polyester is polytetramethylene glycol adipic acid terephthalate, polycaprolactone, polytetramethylene glycol Succinate, polytetramethylene glycol succinic acid adipate ester, polytetramethylene glycol succinic acid terephthalate or PLA.
4. method according to claim 1, it is characterised in that：Step 3) described in compatilizer for glycerin monostearate, OPE, maleic anhydride grafted polyethylene wax, stearic amide, oleamide, ethylene double oleamide, erucic acid acyls The Biodegradable resin of amine, maleic anhydride grafting paraffin or maleic anhydride grafting；Step 3) described in compatilizer consumption be fiber The 1-20% of plain powder consumption, consumption is by weight.
5. method according to claim 1, it is characterised in that：Step 3) described in lubricant be selected from stearic acid, stearic acid Zinc, calcium stearate, Tissuemat E, OPE, paraffin, oxidized paraffin wax, maleic anhydride grafting paraffin or maleic anhydride connect Branch Tissuemat E, step 3) described in lubricant quantity for cellulose powder consumption 0.5-5%, consumption is by weight.
6. method according to claim 1, it is characterised in that：Step 3) described in plasticizer be selected from low mass molecule alcohol chemical combination Thing, the low mass molecule alcohol compound is glycerine or D-sorbite, step 3) plasticizer consumption is for cellulose powder consumption 0.5-5%, consumption is by weight.
7. method according to claim 1, it is characterised in that：Step 3) described in inorganic filler be talcum powder or carbonic acid Calcium；The grain diameter of inorganic filler is less than 50 μm；The consumption of inorganic filler and the ratio of cellulose powder consumption are 0.5：5~10, Consumption is by weight.
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CN111016230A (en) * 2019-12-12 2020-04-17 成都新柯力化工科技有限公司 Method for preparing bio-plastic film by post-inflation stretch blow molding
CN111825958A (en) * 2020-02-26 2020-10-27 上海昶法新材料有限公司 Cellulose-based biodegradable insect-attracting board and preparation method thereof
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CN113480780A (en) * 2021-06-07 2021-10-08 山东路德新材料股份有限公司 Bio-based three-dimensional geonet pad and preparation method thereof
CN114605359A (en) * 2022-03-09 2022-06-10 苏州禾广吉智能装备有限公司 Method for preparing FDCA (fully drawn yarn) and total bio-based filler by using non-grain biomass raw material
CN115746512A (en) * 2022-11-17 2023-03-07 江苏省农业科学院 Method for preparing mulching film based on superfine straw/calcium carbonate powder and product thereof
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CN108250696A (en) * 2017-12-28 2018-07-06 武汉华丽环保科技有限公司 A kind of cellulose complete biodegradable construct blow-molded and preparation method thereof
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CN113429636A (en) * 2021-07-02 2021-09-24 上海经海纬象生物材料有限公司 Full-biodegradable straw reinforced starch material and preparation method thereof
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CN115746512A (en) * 2022-11-17 2023-03-07 江苏省农业科学院 Method for preparing mulching film based on superfine straw/calcium carbonate powder and product thereof

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Application publication date: 20170613