CN103214722B - A kind of easily and the preparation method of polyolefin powder that all mixes of crushed aggregate of plant - Google Patents
A kind of easily and the preparation method of polyolefin powder that all mixes of crushed aggregate of plant Download PDFInfo
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Abstract
The present invention relates to a kind of easily and the polyolefin powder that all mixes of crushed aggregate of plant and preparation method thereof, the composition of powder is polyethylene, polypropylene, polystyrene or their mixture, the particle diameter of powder is 100nm ~ 1mm, apparent density is 0.18g/mL ~ 0.40g/mL, can realize Homogeneous phase mixing with the root of plant, stem, dry, leaf, kind putamen crushed aggregates by mixed media.The precipitation agent thermoprecipitation that the solid materials that the preparation process of powder comprises various form mixes with special solvent, heating for dissolving, use are special, be separated, roll homogenize, break up, be separated solvent and precipitation agent and realize the steps such as recycle, drying, grinding.Whole preparation process has the features such as material cycle utilizes, volatile matter is few, environmental protection property is strong.Prepared powder can be used for preparing environment-friendly composite material, and then manufactures container, furniture, finishing material, toy etc.; Also the raw material that can be used as powder coating and the hot melt adhesion material being easy to even spread.
Description
Technical field
The invention belongs to the special manufacture field of macromolecular material, relate generally to a kind of easily and the preparation method of polyolefin powder that all mixes of crushed aggregate of plant.
Background technology
Polyolefine is the general name of the analog thermoplastic resin obtained by homopolymerization or copolymerization by monomers such as ethene, propylene, 1-butylene, 1-amylene, 1-hexene, 1-octene, 4-methyl-1-pentenes.Due to abundant raw material, cheap, easy machine-shaping, therefore high comprehensive performance is that in macromolecular material, output is maximum, a most widely used kind, and wherein polyethylene, polypropylene, polystyrene are applied particularly extensive.Polyethylene be ethene through being polymerized obtained a kind of thermoplastic resin, odorless, nontoxic, feel ceraceous, has excellent resistance to low temperature, chemical stability, resistance to acids and bases, less water-absorbent, electrical insulating property, is insoluble to common solvent under normal temperature.Polyethylene purposes is very extensive, is mainly used to manufacture film, container, pipeline, electric wire, daily necessities etc., and can be used as the high-frequency insulation material of TV, radar etc.Polypropylene is a kind of thermoplastic synthetic resin of excellent property, has the features such as little, nontoxic, the easy processing of proportion, shock resistance, warp resistance, electrical isolation, has a wide range of applications in automotive industry, household electrical appliance, electronics, packaging and furniture building materials etc.Polystyrene is a kind of water white thermoplastics, has the glass transition temp higher than 100 DEG C, is therefore suitable for the application scenario that temperature requirement is higher.
Polyolefine material excellent property, the convenient sources such as polyethylene, polypropylene, polystyrene.Its application brings great convenience to the production of the mankind, life on the one hand, abandon after using on the other hand and also result in serious environmental pollution in the environment, i.e. " white pollution ", great infringement is brought to agriculture production, halobiontic existence and marine traffic.How to make polyolefinic advantage be not fully exerted, reduce the important content that it is macromolecular material research field to the disadvantageous effect of environment always simultaneously.The reason that polyolefine causes " white pollution " is its refractory organics.For this characteristic, researchist have developed the method for a series of promotion polyolefin products degraded, is included in polyolefine methods such as adding starch, Mierocrystalline cellulose, biodegradation promotor, oxidation promotor.In addition, be one of raw material with polyolefine, being combined the research that the raw material such as the stem of plant, dry, stalk, leaf, root, kind shell prepares advanced composite material also has some to report, and has tempting development prospect.Because for starch, Mierocrystalline cellulose, xylogen, straw, raw material sources such as kind shell, cauline leaf etc. are more convenient, process simpler.The method reporting this kind of matrix material of more preparation in document is extrusion molding.But extrusion molding need few compared with high processing temperature, plant material consumption, need plant material to be processed into the shortcomings such as pulverulence, production efficiency are low, comparatively speaking, adopt pressure sintering to prepare polyolefine/stalk compound material and be easier to scale operation, and there is the advantages such as plant material Morphological adaptability is strong, type of plant material strong adaptability, plant material utilization ratio are high, production environment pollutent discharges less, service temperature is low.
Adopt the excellent polyolefine/stalk compound material of pressure sintering processability to depend on polyolefine and can realize Homogeneous phase mixing with plant material.The polyolefinic raw materials provided in industrial production mainly particulate material, density is large, and plant material has vesicular structure, and density is low.During both mixing, polyolefin pellets is easy to be gathered in bottom, and it is unfavorable to cause to the homogeneity of heat pressing process and material property.Polyolefine materiel machining is become the powder of proper characteristics, be conducive to realizing the Homogeneous phase mixing with crushed aggregate of plant.
Comminuting method is the common method preparing inorganic material powders, but for there is certain technical difficulty during macromolecular material.Because polyolefine has visco-elasticity, be easily out of shape in crushing process, adopt conventional comminuting method often not reach crushing effect, and in crushing process, system can be generated heat, and polyolefine becomes sticky under the action of heat, stop pulverizing effect to be carried out.In order to address this is that, often adopt in production and pulverizing under liquid nitrogen or dry ice cooling effect.Freezing and pulverizing is a kind of mechanical crushing method, needs to consume a large amount of mechanical energy, produces larger noise; Owing to being deep cooling, large with envrionment temperature difference, heat transfer is fast, and refrigerant utilising efficiency is low, and production efficiency is low, easily causes frostbite in operating process, and cold operation proposes higher requirement to equipment.For the shortcoming of current polyolefins powder preparation method, explore the new preparation method of polyolefin powder, be conducive to widening polyolefinic Application Areas, promote the recycling of polyolefine waste material, promote the pressure sintering manufacture of polyolefine/crushed aggregate of plant environment-friendly composite material, new method for preparing raw material can be provided for powder coating, hot melt adhesion material simultaneously.
Summary of the invention
The present invention is conceived to the preparation method widening polyolefin powder, open up the new way that waste polyolefine is recycled, prepare polyolefine/crushed aggregate of plant environment-friendly composite material for pressure sintering and provide excellent property, polyolefin powder material easy to process, simultaneously for powder coating, hot-melt adhesive provide new method for preparing raw material.
The present invention is achieved through the following technical solutions: a kind of polyolefin powder, it is characterized in that, composition is polyethylene, polypropylene, polystyrene or their mixture, the particle diameter of powder is 100nm ~ 1mm, apparent density is 0.18g/mL ~ 0.40g/mL, can realize Homogeneous phase mixing with crushed aggregate of plant by mixed media thing.Crushed aggregate of plant wherein refers to the root of plant, stem, the particle diameter of dry, leaf, kind shell is below 4cm in the powder of below 2mm, length short blank, fiber material, sheet material.The vehicle used when mixing with crushed aggregate of plant is tap water, deionized water, the solid content polymer emulsion below 5%, the polymers soln of solutes content below 2%; The consumption of mixed media thing is that every 100g crushed aggregate of plant uses 8mL ~ 40mL mixed media thing.
Prepare the method for said polyolefins powder, it is characterized in that, comprise the following steps:
S1, by polyolefine material and solvent;
S2, polyolefine is dissolved mixed system reflux;
S3, polyolefinic hot solution is poured in the precipitation agent of stirring;
S4, cooling, suction filtration, rolls repeatedly by filter cake;
S5, by the filter cake rolled by stir, vibration or scraping method be dispersed as Powdered;
S6, powder to be mixed with water, the solvent that underpressure distillation removing is remaining and precipitation agent;
S7, normal pressure or filtration under diminished pressure, isolate solvent-free, without the polyolefine wet powder of precipitation agent;
S8, by polyolefine wet powder by dry in the air, shine or the oven heating of less than 70 DEG C dry, then grind;
S9, the filtrate in above-mentioned steps S4 to be mixed with polyolefine, suitably supplement the solvent lost in treating processes, then distill, to polyolefine dissolves, the hot solution obtained enters the process from above-mentioned steps S3, and the material distilled out recycles as the precipitation agent in step S3; Distillate in above-mentioned steps S6 is carried out separatory, and oil phase uses as solvent cycle;
In addition in said process, solvent is toluene, dimethylbenzene or their mixture, and precipitation agent is dehydrated alcohol.
As preferably of the present invention, in step sl, polyolefine material refers to the material of particulate material, block material or other non-powder morphology; The consumption of solvent is per kilogram polyolefine, throws 10 liters ~ 50 liters solvents.In step s 2, the bath temperature of heating is 120 DEG C ~ 200 DEG C; In step s3, the temperature of polyolefine hot solution is 85 DEG C ~ 140 DEG C, and precipitation agent is dehydrated alcohol, precipitation agent and solvent be that often liter of solvent need use precipitation agent 0.7 liter ~ 5 liters with magnitude relation.In step s 6, the consumption of water is that per kilogram polyolefin powder uses 5 liters ~ 50 premium on currency; Must stir during underpressure distillation; The bath temperature of underpressure distillation is 85 DEG C ~ 97 DEG C.
The polyolefin powder prepared in the present invention has a wide range of applications, and as the raw material of hot melt adhesive, can be used in the bonding aspect of cloth, paper etc., also can as the raw material of thermoplastic powder coating or the modifying material as powder coating.In addition, after polyolefine is become powder, the weight saving of particle, be conducive to light material with other and realize Homogeneous phase mixing, for mixing, this requires that higher application scenario has great importance, such as can realize mixing, to prepare their matrix material of polyolefine and plant straw powder or vegetable fibre easily.Prepared matrix material mating surface coating technology can be used for manufacturing packaging vessel, furniture, finishing material, show and colour, cast material, toy etc.
The present invention have employed the method for thermoprecipitation in step s3, enhances polyolefine solvability in a solvent, decreases the usage quantity of solvent, is conducive to obtaining that particle is comparatively thin, the good powder of mobility.The present invention adopts the material containing solvent and precipitation agent in step s 4 which and repeatedly rolls process, is conducive to increasing the form of powder and the homogeneity of size, follow-up step of breaing up more easily is carried out.The present invention in step s 6, when separatory distillation is carried out to the powder containing solvent and precipitation agent, carry out of system temperature on the coalescent of powder and still-process has very important impact, temperature is too high very easily forms irreversible agglomerate, temperature is too low, and vacuum condition requires high, and kinetic energy consumption is large, and solvent loss is large, recovery utilization rate is low.Powder preparation method proposed by the invention, has caught the key condition window of each step, whole process smoothness, circulation, reliable, environmental protection.
For freezing and pulverizing method, the feature such as that the preparation method of polyolefin powder of the present invention has that noise is low, easy and simple to handle, operation material recycles, solvent volatilizees in environment is less, the feature of environmental protection is strong.Freezing and pulverizing method belongs to dry method powder process, and the present invention then belongs to wet powder-making.Although the present invention employs solvent, solvent can recycle, less consumption solvent; Although employ solvent, not containing solvent in powder-product, ensure that the security of powdered material; Although employ organic solvent, process can carry out in the system of airtight or semi closed in steps, decrease scattering and disappearing of organic solvent as far as possible.The solvent used in process and precipitation agent can reclaim, and recycle, and have embodied obvious greenization feature.
The preparation method of the polyolefin powder in the present invention is not only applicable to new grain material, and is applicable to the waste or used plastics of recovery.The macromolecular material comprising plastics is the material type that volumetric production is maximum in the world.Output also just determines greatly with rear discarded in the environment more, thus causes serious white pollution.In order to reduce the harm of white pollution, a lot of country proposes plastic limit in the world.But plastic limit fundamentally can not solve white pollution, solution route fundamentally makes polyolefine degradable or recycles.The preparation method of polyolefin powder of the present invention is a kind of method of technics of reclaim of plastic waste simultaneously, to development low-carbon economy, promotes human health, promotes that ecological economic development is significant.
The approach widely usedly at present to reclaim polyolefine waste material, be processed into easy-to-use form makes regenerated granule by extruding pelletization legal system.Extrusion molding belongs to hot melt working method, and all waste materials all enter regenerated granule, and product composition is complicated, and service temperature is high, and production environment stink is large.In polyolefine waste recovery, method of the present invention is solution processing method, and service temperature is low; Owing to have employed solvent system, some impurity component in plastic waste can by the method removing be separated, and the reworked material obtained is purer.
Accompanying drawing explanation
Fig. 1 is the apparent density of polyethylene powders and the contrast of the apparent density with polyethylene particle prepared by the specific embodiment of the invention 1.
Fig. 2 for by the specific embodiment of the invention 1, but changes the consumption of precipitation agent, the rule that the apparent density after prepared polyethylene powders jolt ramming changes with the volume ratio of precipitation agent and solvent.
Fig. 3 for by the specific embodiment of the invention 1, but changes the consumption of precipitation agent, the rule that screenings when prepared polyethylene powders uses 20 mesh sieves screening changes with the volume ratio of precipitation agent and solvent.
Fig. 4 is the tensile strength using the matrix material prepared by pressure sintering by polyethylene powders and the crushed aggregates of straw of the specific embodiment of the invention 1 preparation, the rule changed with the change of the percentage ratio of polyethylene powders in straw and polyethylene powders total mass.
Embodiment
Embodiment 1
1 kilogram of polyethylene pellet and 15 liters of dimethylbenzene are loaded return stirring heating kettle, under agitation system is warmed up to 140 DEG C, and reflux under this temperature condition until polyethylene dissolves.After making system temperature be down to 100 DEG C, slowly pour being equipped with in the mixing kettle of 15 liters of dehydrated alcohols of stirring into, be finished down rear enclosed and stir, until system is down to room temperature.By the material decompress filter in mixing kettle, filter cake is rolled by stone mill, then dryly stirs powdered.Gained powder is loaded in underpressure distillation still, adds 10 liters of tap water simultaneously, be warming up to 95 DEG C under agitation, reduce pressure with water pump, gradually Raise vacuum degree, guarantee that still-process steadily carries out, until no longer including till dimethylbenzene steams.Material decompress filter in still, filtrate is reused as distillation water, and solid polyolefin powder dries.
Fig. 1 is the apparent density of polyethylene powders and the contrast of the apparent density with polyethylene particle prepared by the specific embodiment of the invention 1.As seen from the figure, the apparent density of polyethylene powders declines to a great extent than the apparent density of polyethylene particle, and before and after jolt ramming, the apparent density of polyethylene powders does not have considerable change.
Fig. 2 for by the specific embodiment of the invention 1, but changes the consumption of precipitation agent, the rule that the apparent density after prepared polyethylene powders jolt ramming changes with the volume ratio of precipitation agent and solvent.As seen from the figure, with the increase of precipitation agent consumption, the apparent density of polyethylene powders presents the rear trend stably of first minimizing.Precipitation agent consumption easily forms agglomerating particles time few, and can form fine uniform particle when precipitation agent consumption is large, precipitation agent consumption acquires a certain degree, and impact reduces.
Fig. 3 for by the specific embodiment of the invention 1, but changes the consumption of precipitation agent, the rule that screenings when prepared polyethylene powders uses 20 mesh sieves screening changes with the volume ratio of precipitation agent and solvent.As seen from the figure, with the increase of precipitation agent consumption, polyethylene powders 20 mesh sieve screenings reduces gradually, shows that precipitation agent consumption is conducive to greatly reducing polyethylene powders and reunites, prevents from forming macrobead.
Fig. 4 is the tensile strength using the matrix material prepared by pressure sintering by polyethylene powders and the crushed aggregates of straw of the specific embodiment of the invention 1 preparation, the rule changed with the change of the percentage ratio of polyethylene powders in straw and polyethylene powders total mass.As seen from the figure, with the increase of polyethylene powders consumption, straw is bonding more abundant, and the tensile strength of matrix material increases gradually.But when polyethylene consumption is excessive, excessively can assemble in the composite, and form new textural defect, cause matrix material tensile strength to decrease.
Embodiment 2
1 kilogram of recycle polyethylene film and bottle material and 20 liters of toluene are loaded return stirring heating kettle, under agitation system are warmed up to 160 DEG C, and under this temperature condition backflow until polyethylene dissolves.After making system temperature be down to 110 DEG C, the impurity of surface flotation is removed in drift, and that slowly pours stirring into is equipped with in the mixing kettle of 35 liters of dehydrated alcohols, makes bottom settlings impurity be retained in return stirring heating kettle when toppling over.Be finished down rear enclosed to stir, until system is down to room temperature.By the material decompress filter in mixing kettle, filter cake is rolled by stone mill, then stirs powdered with four leaf bar type stirring devices are dry.Gained powder is loaded in underpressure distillation still, adds 20 liters of tap water simultaneously, be warming up to 95 DEG C under agitation, reduce pressure with water pump, gradually Raise vacuum degree, guarantee that still-process steadily carries out, until no longer including till dimethylbenzene steams.Material natural filtration in still, filtrate is reused as distillation water, and solid polyolefin powder is done to constant weight in 50 DEG C of baking ovens.
Embodiment 3
1 kilogram of recycle polyethylene, polystyrene, polyacrylic hybridization film and bottle material and 10 liters of toluene, 10 liters of dimethylbenzene are loaded return stirring heating kettle, under agitation system is warmed up to 160 DEG C, and reflux under this temperature condition until polyethylene dissolves.After making system temperature be down to 110 DEG C, the impurity of surface flotation is removed in drift, and that slowly pours stirring into is equipped with in the mixing kettle of 40 liters of dehydrated alcohols, makes bottom settlings impurity be retained in return stirring heating kettle when toppling over.Be finished down rear enclosed to stir, until system is down to room temperature.By the material decompress filter in mixing kettle, filter cake is rolled by stone mill, then dryly stirs powdered.Gained powder is loaded in underpressure distillation still, adds 15 liters of tap water simultaneously, be warming up to 96 DEG C under agitation, reduce pressure with water pump, gradually Raise vacuum degree, guarantee that still-process steadily carries out, until no longer including toluene, till dimethylbenzene steams.Material decompress filter in still, filtrate is reused as distillation water, and solid polyolefin powder is dried at 50 DEG C.
Embodiment 4
The composite grain material of 1 kilogram of polyethylene, polystyrene and 5 liters of toluene, 25 liters of dimethylbenzene are loaded return stirring heating kettle, under agitation system is warmed up to 180 DEG C, and reflux under this temperature condition until polyethylene dissolves.After making system temperature be down to 120 DEG C, slowly pour being equipped with in the mixing kettle of 50 liters of dehydrated alcohols of stirring into, be finished down rear enclosed and stir, until system is down to room temperature.By the material decompress filter in mixing kettle, filter cake is rolled by stone mill, then dryly stirs powdered.Gained powder is loaded in underpressure distillation still, adds 7 liters of tap water simultaneously, be warming up to 94 DEG C under agitation, reduce pressure with water pump, gradually Raise vacuum degree, guarantee that still-process steadily carries out, until no longer including toluene, till dimethylbenzene steams.Material decompress filter in still, filtrate is reused as distillation water, and solid polyolefin powder dries.
Claims (5)
1. one kind easily and the preparation method of polyolefin powder that all mixes of crushed aggregate of plant, described polyolefin powder composition is any one or two or more mixtures of polyethylene, polypropylene, polystyrene, the particle diameter of powder is 100nm ~ 1mm, apparent density is 0.18g/mL ~ 0.40g/mL, Homogeneous phase mixing can be realized by mixed media thing with crushed aggregate of plant, it is characterized in that, comprise the following steps:
S1, by polyolefine material and solvent;
S2, polyolefine is dissolved mixed system reflux;
S3, polyolefinic hot solution is poured in the precipitation agent of stirring;
S4, cooling, suction filtration, rolls repeatedly by filter cake;
S5, by the filter cake rolled by stir, vibration or scraping method be dispersed as Powdered;
S6, powder to be mixed with water, the solvent that underpressure distillation removing is remaining and precipitation agent;
S7, normal pressure or filtration under diminished pressure, isolate solvent-free, without the polyolefine wet powder of precipitation agent;
S8, by polyolefine wet powder by dry in the air, shine or the oven heating of less than 70 DEG C dry, then grind;
S9, the filtrate in above-mentioned steps S4 to be mixed with polyolefine, suitably supplement the solvent lost in treating processes, then distill, to polyolefine dissolves, the hot solution obtained enters the process from above-mentioned steps S3, and the material distilled out recycles as the precipitation agent in step S3; Distillate in above-mentioned steps S6 is carried out separatory, and oil phase uses as solvent cycle;
Solvent described in above step is toluene, dimethylbenzene or their mixture; Described precipitation agent is dehydrated alcohol.
2. the preparation method of polyolefin powder according to claim 1, is characterized in that, in step sl, polyolefine material refers to the material of particulate material, block material or other non-powder morphology; The consumption of solvent is per kilogram polyolefine, throws 10 liters ~ 50 liters solvents.
3. the preparation method of polyolefin powder according to claim 1, is characterized in that, in step s 2, the bath temperature of heating is 120 DEG C ~ 200 DEG C.
4. the preparation method of polyolefin powder according to claim 1, is characterized in that, in step s3, the temperature of polyolefine hot solution is 85 DEG C ~ 140 DEG C, precipitation agent and solvent be that often liter of solvent need use precipitation agent 0.7 liter ~ 5 liters with magnitude relation.
5. the preparation method of polyolefin powder according to claim 1, in step s 6, the consumption of water is that per kilogram polyolefin powder uses 5 liters ~ 50 premium on currency; Must stir during underpressure distillation; The bath temperature of underpressure distillation is 85 DEG C ~ 97 DEG C.
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| CN103483844B (en) * | 2013-09-10 | 2015-07-22 | 九江学院 | Method for preparing polyethylene and plant composite material |
| US20170251824A1 (en) | 2016-03-07 | 2017-09-07 | Purple Innovation, Llc | Cushions including a coated elastomeric cushioning element and related methods |
| CN107793813A (en) * | 2017-09-28 | 2018-03-13 | 浙江瀚镪自动化设备股份有限公司 | A kind of preparation method of microthin coating powdery paints for automation equipment |
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| CN101665601A (en) * | 2008-09-02 | 2010-03-10 | 住友化学株式会社 | Process for producing organic fiber-containing polyolefin resin composition |
| CN102070911A (en) * | 2010-11-23 | 2011-05-25 | 成都芝田高分子材料有限公司 | Polyolefin/vegetable fiber composite material and preparation method thereof |
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| CN101665601A (en) * | 2008-09-02 | 2010-03-10 | 住友化学株式会社 | Process for producing organic fiber-containing polyolefin resin composition |
| CN102070911A (en) * | 2010-11-23 | 2011-05-25 | 成都芝田高分子材料有限公司 | Polyolefin/vegetable fiber composite material and preparation method thereof |
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