A kind of preparation method of fused glass pellet polylactic acid composite wire

文档序号:1751020 发布日期:2019-11-29 浏览:23次 中文

阅读说明:本技术 一种熔融沉积成型用聚乳酸复合线材的制备方法 (A kind of preparation method of fused glass pellet polylactic acid composite wire ) 是由 许民 韩丽娜 李亚兰 王福华 孟现允 石艳梅 沈欢 庄凯侠 魏鹏 于 2019-08-23 设计创作,主要内容包括:本发明公开了一种熔融沉积成型用聚乳酸复合线材的制备方法,包括;本发明中的一种熔融沉积成型用聚乳酸复合线材的制备方法,现有的3D打印材料采用生物质聚合物复合材料的很少,且生物降解性有待加强,本发明所述的熔融沉积成型用麦秸粉/聚乳酸复合线材打印的制品具有木质感,原料麦秸粉与聚乳酸都完全生物可降解,不会对环境造成任何污染,并且麦秸粉的加入大大加速了材料的降解速率,符合绿色环保的生态理念,且打印的制品防腐防霉,也可以在一定程度上起到节约成本的作用。(The invention discloses a kind of fused glass pellet preparation methods of polylactic acid composite wire, including;The preparation method of one of present invention fused glass pellet polylactic acid composite wire, existing 3D printing material is seldom using biomass polymers composite material, and biological degradability have it is to be strengthened, fused glass pellet of the present invention has woodiness touch with wheat straw powder/polylactic acid composite wire printing product, raw material wheat straw powder and all complete biodegradable of polylactic acid, any pollution will not be caused to environment, and the addition of wheat straw powder has greatly accelerated the degradation rate of material, meet environmentally protective Ecological Concept, and the product anticorrosion of printing is mould proof, it can also play the role of save the cost to a certain extent.)

1. a kind of fused glass pellet preparation method of polylactic acid composite wire, which is characterized in that former including following parts by weight Material: 0.1-15 parts of wheat straw powder, 85-109 parts of polylactic acid, 0.001-1.4 parts of coupling agent, 0.05-2.5 parts of compatilizer, lubricant 0.02-2 parts.

2. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In, including following raw material: 1-5 parts of wheat straw powder, 95-99 parts of polylactic acid, 0.02-0.4 parts of coupling agent, compatilizer 0.5- 1.5 parts, 0.2-1 parts of lubricant.

3. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In the partial size of the wheat straw powder is 100-120 mesh.

4. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In the polylactic acid is the condensation polymer of lactic acid or lactide.

5. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In, the coupling agent be silane coupling agent, titanate coupling agent, aluminate coupling agent, lignin coupling agent, in tin coupling agent At least one.

6. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In, the compatilizer is maleic anhydride grafted polyethylene copolymer, at least one in maleic anhydride inoculated polypropylene copolymer Kind.

7. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In the lubricant is at least one of polyethylene wax, paraffin.

8. a kind of preparation method of fused glass pellet polylactic acid composite wire according to claim 1, feature exist In preparation method is as follows:

The screening of step 1, wheat straw powder: wheat straw powder first passes through 100 the polished standard screens removal coarse powder material, then passes through the mark of 120 mesh Standard is weeded out except fine powder material, finally obtains partial size in the wheat straw powder powder of 100-120 mesh;

The hydrolysis of step 2, coupling agent: 95% ethyl alcohol that parts by weight are 5-15 parts is weighed, the pH value of ethyl alcohol is adjusted with acetic acid It is spare in 3-4, the coupling agent that parts by weight are 0.02-0.4 parts is weighed, load weighted coupling agent is instilled into second under agitation In alcoholic solution, rate of addition is 60-150 drop/min, mixing speed 300-500rad/min, mixing time 1-6h, to idol Connection agent is fully hydrolyzed rear spare;

The modification of step 3, wheat straw powder: weighing the wheat straw powder powder that the step 1 that parts by weight are 1-5 parts obtains, will be load weighted Wheat straw powder powder pours into high-speed mixer, and the coupling agent solution hydrolyzed at 60 DEG C with step 2 sprays wheat straw powder, spray Continue to stir 10-30min, mixing speed 1000-5000rad/min after leaching, wheat straw powder is taken out after stirring in room temperature Under hang 6-12h, be then placed in baking oven at 80-105 DEG C it is dry for 24 hours, it is spare after natural cooling;

The mixing of step 4, raw material: it is by the modified wheat straw powder of step 3, the polylactic acid that parts by weight are 95-99 parts, parts by weight Mixed at high speed, mixing are fast in a high speed mixer for 0.5-1.5 parts of compatilizer, the lubricant that parts by weight are 0.2-1 parts 1000-5000rad/min is spent, mixing time 30-60min obtains uniformly mixed material;

The preparation of step 5, pellet: material melting extrusion in double screw extruder that step 4 is uniformly mixed, the ginseng of extruder Number setting are as follows: 152-160 DEG C of area's temperature, two 162-170 DEG C of area's temperature, three 165-175 DEG C of area's temperature, four area temperature 175- 180 DEG C, five 175-180 DEG C of area's temperature, six 172-180 DEG C of area's temperature, seven 165-175 DEG C of area's temperature, powder after melt extrusion is cooling Broken obtained pellet;

Step 6, wire-drawing shape: pellet made from step 5 is added to high-accuracy 3D printing consumptive material extrusion test machine, carries out wire drawing Molding, the parameter setting of wire-drawing shape extruder are as follows: 35-45 DEG C of water temperature, 160-170 DEG C of one area of barrel, two area 165-175 of barrel DEG C, 165-175 DEG C of mold, host speed is set as 30-50Hz, and hauling speed is set as 20-30Hz, obtains fused glass pellet With wheat straw powder composite wire.

Technical field

The present invention relates to polylactic acid composite wire technical fields, multiple with polylactic acid more particularly to a kind of fused glass pellet The preparation method of zygonema material.

Background technique

Currently, the importance of 3D printing has been verified, and it is widely used in industry.Existing particulate metal powder The materials such as end are primarily adapted for use in the 3D printing of technical grade and expensive, can be used for household 3D printing material be only limitted to gypsum, Resin, plastics etc., are far from satisfying the market demand.In numerous 3D printing techniques, fused glass pellet (FDM) technology is the most Common, device structure is simple, cheap, and operating procedure is convenient, and print procedure is to spray thermoplasticity filamentary material from heating It melts in mouth, and squeezes out according to the track of design to construct 3D solid.Obviously, it proposes more to can be used for the novel of 3D printing Composite material has very big market prospects, and the material bottleneck for solving 3D printing has important value.With country It is more and more to environmentally protective proposition to require, it is necessary to prepare complete biodegradable 3D printing material, avoiding can not The waste of regenerated resources.In recent years, biomass polymers composite material not only had as a kind of special green material The mould proof advantage of plastic anti-corrosion, there are also special woodiness touch.As one kind of biomass polymers composite material, wheat moulds composite wood Material, mainly using plastics as matrix, wheat straw powder is used as reinforcement in the base to improve the mechanical property of system.Wheat straw money Source is abundant, can be degradable, is used for the preparation of FDM type 3D printing material, not only can solve wheat straw and largely arbitrarily fired It burns to the problem of environmental pollution of the Northeast's bring, also there is definite meaning for developing wheat straw economy.

Therefore, in view of the above technical problems, it is necessary to which a kind of system of fused glass pellet polylactic acid composite wire is provided Preparation Method.

Summary of the invention

In view of this, the purpose of the present invention is to provide a kind of preparation sides of fused glass pellet polylactic acid composite wire Method, existing 3D printing material is seldom using biomass polymers composite material, and biological degradability has to be strengthened, the present invention The fused glass pellet product of wheat straw powder/polylactic acid composite wire printing has a woodiness touch, raw material wheat straw powder and poly- The all complete biodegradable of lactic acid will not cause any pollution to environment, and the addition of wheat straw powder has greatly accelerated material Degradation rate meets environmentally protective Ecological Concept, and the product anticorrosion printed is mould proof, can also play section to a certain extent The about effect of cost.

To achieve the goals above, the technical solution that one embodiment of the invention provides is as follows:

A kind of preparation method of fused glass pellet polylactic acid composite wire, including following raw material: wheat straw powder 0.1-15 parts, 85-109 parts of polylactic acid, 0.001-1.4 parts of coupling agent, 0.05-2.5 parts of compatilizer, 0.02-2 parts of lubricant.

As a further improvement of the present invention, including following raw material: 1-5 parts of wheat straw powder, 95-99 parts of polylactic acid, 0.02-0.4 parts of coupling agent, 0.5-1.5 parts of compatilizer, 0.2-1 parts of lubricant.

As a further improvement of the present invention, the partial size of the wheat straw powder is 100-120 mesh.

As a further improvement of the present invention, the polylactic acid is the condensation polymer of lactic acid or lactide.

As a further improvement of the present invention, the coupling agent is silane coupling agent, titanate coupling agent, Aluminate idol Join agent, lignin coupling agent, at least one of tin coupling agent.

As a further improvement of the present invention, the compatilizer is maleic anhydride grafted polyethylene copolymer, maleic acid At least one of acid anhydride graft polypropylene copolymer.

As a further improvement of the present invention, the lubricant is at least one of polyethylene wax, paraffin.

As a further improvement of the present invention, preparation method is as follows:

The screening of step 1, wheat straw powder: wheat straw powder first passes through 100 the polished standard screens removal coarse powder material, then passes through 120 mesh Standard screen remove fine powder material, finally obtain partial size 100-120 mesh wheat straw powder powder;

The hydrolysis of step 2, coupling agent: weighing 95% ethyl alcohol that parts by weight are 5-15 parts, adjusts ethyl alcohol with acetic acid PH value is spare in 3-4, weighs the coupling agent that parts by weight are 0.02-0.4 parts, load weighted coupling agent is dripped under agitation Enter in ethanol solution, rate of addition be 60-150 drop/min, mixing speed 300-500rad/min, mixing time 1-6h, It is spare after coupling agent is fully hydrolyzed;

The modification of step 3, wheat straw powder: the wheat straw powder powder that the step 1 that parts by weight are 1-5 parts obtains is weighed, will be weighed Good wheat straw powder powder pours into high-speed mixer, and the coupling agent solution hydrolyzed at 60 DEG C with step 2 sprays wheat straw powder Leaching, continues after spray to stir 10-30min, mixing speed 1000-5000rad/min, taken out after stirring wheat straw powder in 6-12h is hung at room temperature, and it is for 24 hours, spare after natural cooling to be then placed in baking oven drying at 80-105 DEG C;

The mixing of step 4, raw material: by the modified wheat straw powder of step 3, the polylactic acid that parts by weight are 95-99 parts, parts by weight Compatilizer that number is 0.5-1.5 parts, the lubricant that parts by weight are 0.2-1 parts in a high speed mixer stir by mixed at high speed, mixing Speed 1000-5000rad/min is mixed, mixing time 30-60min obtains uniformly mixed material;

The preparation of step 5, pellet: material melting extrusion in double screw extruder that step 4 is uniformly mixed, extruder Parameter setting are as follows: 152-160 DEG C of area's temperature, two 162-170 DEG C of area's temperature, three 165-175 DEG C of area's temperature, four Qu Wendu 175-180 DEG C, five 175-180 DEG C of area's temperature, six 172-180 DEG C of area's temperature, seven 165-175 DEG C of area's temperature, melt, which squeezes out, to be cooled down It crushes afterwards and pellet is made;

Step 6, wire-drawing shape: being added to high-accuracy 3D printing consumptive material extrusion test machine for pellet made from step 5, carries out Wire-drawing shape, the parameter setting of wire-drawing shape extruder are as follows: 35-45 DEG C of water temperature, 160-170 DEG C of one area of barrel, 2nd area of barrel 165-175 DEG C, 165-175 DEG C of mold, host speed is set as 30-50Hz, and hauling speed is set as 20-30Hz, is melted Deposition modeling wheat straw powder composite wire.

The beneficial effects of the present invention are: the preparation side of one of present invention fused glass pellet polylactic acid composite wire Method, existing 3D printing material is seldom using biomass polymers composite material, and biological degradability has to be strengthened, the present invention The fused glass pellet product of wheat straw powder/polylactic acid composite wire printing has a woodiness touch, raw material wheat straw powder and poly- The all complete biodegradable of lactic acid will not cause any pollution to environment, and the addition of wheat straw powder has greatly accelerated material Degradation rate meets environmentally protective Ecological Concept, and the product anticorrosion printed is mould proof, can also play section to a certain extent The about effect of cost.

Detailed description of the invention

In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The some embodiments recorded in invention, for those of ordinary skill in the art, without creative efforts, It is also possible to obtain other drawings based on these drawings.

Fig. 1 is present invention process flow diagram;

Fig. 2 is degradation speed curve of the present invention under different concentration of lye;

Fig. 3 is fused glass pellet schematic diagram of the present invention;

Fig. 4 is degradation speed curve of the pure polylactic acid wire rod under different concentration of lye.

Specific embodiment

Technical solution in order to enable those skilled in the art to better understand the present invention, below in conjunction with of the invention real The attached drawing in example is applied, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common Technical staff's every other embodiment obtained without making creative work, all should belong to protection of the present invention Range.

In each diagram of the invention, for the ease of illustration, structure or partial certain sizes can be relative to other knots Therefore structure or partial enlargement are only used for the basic structure of diagram subject of the present invention.

The term of the representation space relative position used herein such as "left", "right", " left side ", " right side " is for just A unit as shown in the drawings or feature are described relative to another unit or the relationship of feature in the purpose of explanation.It is empty Between the term of relative position can be intended to include different direction of the equipment in use or work other than orientation as shown in the figure. For example, the unit for being described as being located at other units or feature " right side " will be located at other if the equipment in figure overturn Unit or feature " left side ".Therefore, exemplary term " right side " can include both orientation of left and right side.Equipment can be with Other modes are directed (be rotated by 90 ° or other directions), and are interpreted accordingly used herein with space correlation description language.

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