CN114773806B - Degradable composite material for thin-wall injection molding and preparation method thereof - Google Patents
Degradable composite material for thin-wall injection molding and preparation method thereof Download PDFInfo
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a degradable composite material for thin-wall injection molding, which comprises the following components: 30-80 parts of biodegradable resin, 10-50 parts of flexibilizer, 1-5 parts of flow promoter, 5-20 parts of degradable glass fiber, 1-5 parts of fiber surface treating agent, 1-5 parts of compatibilizer, 5-20 parts of inorganic filling material, 0.2-1 part of heat-resistant modification assistant and 0.1-0.8 part of lubricant by mass. The degradable composite material disclosed by the invention is completely biodegradable in formula, is environment-friendly, has excellent flowability, temperature resistance and mechanical property, and is suitable for preparing thin-wall injection molding products.
Description
Technical Field
The invention belongs to the technical field of biodegradable composite materials, and particularly relates to a degradable composite material for thin-wall injection molding, and further relates to a preparation method of the degradable composite material for thin-wall injection molding.
Background
At present, along with the change of life style of people, the demands for takeaway are increasingly increased, takeaway cutlery box is mixed with food residues, and is difficult to clean, so that cutlery box products cannot be effectively recycled, and meanwhile, the traditional polypropylene cutlery box cannot be composted and degraded, so that larger resource waste and serious environmental pollution are caused. The degradable takeaway cutlery box uses environment-friendly materials, can be composted and degraded together with food residues when being discarded, and can simultaneously meet the common requirements of people on convenient life style and environmental protection.
The wall thickness of the injection molding cutlery box product is different from 0.3mm to 0.6mm, the wall thickness of the product is small, the requirement on the fluidity of the material is higher, the brittleness of the material can be obviously increased under the condition of thinner wall thickness, and meanwhile, the cutlery box is required to have certain heat resistance when containing food. The existing biodegradable materials are difficult to meet the use requirements in all aspects. Therefore, there is a need for research improvements in current biodegradable materials.
Disclosure of Invention
The present invention has been made based on the findings and knowledge of the inventors regarding the following facts and problems: in the related art, CN112694727A discloses a biodegradable material, the fluidity of which is insufficient and can only reach 55g/10min; CN113185809a discloses a biodegradable composite material, and because glycerol epoxy resin is adopted in the composite material, there is a risk of difficult complete biodegradation.
The present invention aims to solve at least one of the technical problems in the related art to some extent. Therefore, the embodiment of the invention provides the degradable composite material for thin-wall injection molding, and the degradable material is fully adopted in the formula, so that the composite material can be completely biodegraded, is environment-friendly, has excellent fluidity, temperature resistance and mechanical properties, and is suitable for preparing thin-wall injection molding products.
The embodiment of the invention provides a degradable composite material for thin-wall injection molding, which comprises the following components: 30-80 parts of biodegradable resin, 10-50 parts of toughening agent, 1-5 parts of flow promoter, 5-20 parts of degradable glass fiber, 1-5 parts of fiber surface treatment agent, 1-5 parts of compatilizer, 5-20 parts of inorganic filling material, 0.2-1 part of heat-resistant modification auxiliary agent and 0.1-0.8 part of lubricant by mass.
The degradable composite material for thin-wall injection molding provided by the embodiment of the invention has the advantages and technical effects that 1, in the embodiment of the invention, the adopted matrix material is biodegradable resin, and the adopted other raw materials also belong to the degradable material, so that the composite material can realize complete biodegradation; 2. in the embodiment of the invention, the plasticizing effect of the two materials, namely the flow promoter and the fiber surface treating agent, on the biodegradable resin is utilized, the regulation and control on the fluidity of the composite material are effectively realized, the melt flow rate of the composite material can be controlled to be 60-120g/10min, and the processing requirement of thin-wall injection molding can be completely met; 3. in the embodiment of the invention, the heat-resistant modified auxiliary agent and the degradable glass fiber are used cooperatively, so that the temperature resistance and the mechanical property of the composite material are effectively improved.
In some embodiments, the biodegradable resin comprises polylactic acid, and the biodegradable resin has a weight average molecular weight of 8 ten thousand to 30 ten thousand.
In some embodiments, the toughening agent is a flexible biodegradable resin comprising at least one of polybutylene succinate, polybutylene succinate-adipate-butylene succinate; the flow promoter is low molecular weight polylactic acid with a molecular weight of 2000-8000.
In some embodiments, the fiber surface treatment is polyethylene glycol.
In some embodiments, the degradable glass fiber comprises:
In some embodiments, the inorganic filler material comprises at least one of talc, calcium carbonate, montmorillonite; the lubricant comprises at least one of erucamide, oleamide and wax substances.
In some embodiments, the compatibilizing agent is a polyethylene glycol/lactic acid copolymer.
In some embodiments, the heat resistant modifying aid is an aromatic sulfonate derivative.
The embodiment of the invention also provides a preparation method of the degradable composite material for thin-wall injection molding, which comprises the following steps:
a. pretreatment of degradable glass fibers: firstly, putting degradable glass fiber and a fiber surface treating agent together in a mixer, and fully mixing;
b. And d, mixing the biodegradable resin, the toughening agent, the flow promoter, the compatilizer, the inorganic filling material, the heat-resistant modification auxiliary agent and the lubricant according to a designed proportion, adding the mixture into a double-screw extruder, adding the glass fiber pretreated in the step a in a side feeding mode, and carrying out co-extrusion granulation in the double-screw extruder to obtain the degradable composite material.
The preparation method of the degradable composite material for thin-wall injection molding provided by the embodiment of the invention has the advantages and technical effects of simple preparation process, capability of being directly processed by common equipment, easiness in industrial application, good fluidity of the prepared composite material, excellent temperature resistance and mechanical property, and capability of meeting the requirements of thin-wall injection molding products.
In some embodiments, in step a, the mixer temperature is controlled to 60-80 ℃; in the step b, the extrusion temperature is 150-190 ℃.
Detailed Description
The following detailed description of embodiments of the invention is exemplary and intended to be illustrative of the invention and not to be construed as limiting the invention.
The embodiment of the invention provides a degradable composite material for thin-wall injection molding, which comprises the following components: 30-80 parts of biodegradable resin, 10-50 parts of toughening agent, 1-5 parts of flow promoter, 5-20 parts of degradable glass fiber, 1-5 parts of fiber surface treatment agent, 1-5 parts of compatilizer, 5-20 parts of inorganic filling material, 0.2-1 part of heat-resistant modification auxiliary agent and 0.1-0.8 part of lubricant by mass.
The degradable composite material for thin-wall injection molding provided by the embodiment of the invention adopts the matrix material as the biodegradable resin, and other adopted raw materials also belong to the degradable material, so that the composite material can be completely biodegraded; in the embodiment of the invention, the plasticizing effect of the two materials, namely the flow promoter and the fiber surface treating agent, on the biodegradable resin is utilized, the regulation and control on the fluidity of the composite material are effectively realized, the melt flow rate of the composite material can be controlled to be 60-120g/10min, and the processing requirement of thin-wall injection molding can be completely met; in the embodiment of the invention, the heat-resistant modified auxiliary agent and the degradable glass fiber are used cooperatively, so that the temperature resistance and the mechanical property of the composite material are effectively improved.
In some embodiments, the biodegradable resin comprises polylactic acid, the biodegradable resin having a weight average molecular weight of 8-30 ten thousand; the toughening agent is flexible biodegradable resin and comprises at least one of poly (butylene succinate) and poly (succinic acid-adipic acid-butylene succinate); the flow promoter is low molecular weight polylactic acid with a molecular weight of 2000-8000. In the embodiment of the invention, all the adopted raw materials are degradable raw materials, so that the prepared composite material can be completely biodegraded. In addition, the embodiment of the invention adds the low molecular weight polylactic acid as the flow promoter, thereby effectively increasing the plasticity of the biodegradable resin and improving the fluidity of the composite material.
In some embodiments, the fiber surface treatment agent is polyethylene glycol, preferably PEG400; the compatilizer is polyethylene glycol/lactic acid copolymer. In the embodiment of the invention, polyethylene glycol is preferably used as a surface treatment agent of the glass fiber, has good polarity, can be well combined with the polar surface of the glass fiber, and can fully infiltrate the glass fiber bundles as a liquid material. In addition, polyethylene glycol and a compatilizer can synergistically act, and because the surface of the glass fiber is treated by polyethylene glycol, when the polyethylene glycol/lactic acid copolymer is used as the compatilizer, the ethylene glycol chain segment in the compatilizer can be fully combined with the polyethylene glycol on the surface of the glass fiber, and the rest lactic acid chain segments in the compatilizer can be fully combined with the polylactic acid of the biodegradable resin, so that the effect of increasing the bonding strength of the glass fiber and the polylactic acid of the biodegradable resin is achieved. Therefore, the polyethylene glycol is mainly used as a surface treatment agent of the glass fiber, and under the synergistic effect of the compatilizer, the interfacial binding force between the glass fiber and the biodegradable resin polylactic acid is enhanced, so that the performance of the composite material is enhanced; meanwhile, because the polyethylene glycol (PEG 400) is in a liquid state and has smaller molecular weight, the plasticizing effect can be achieved in the composite material, thereby promoting the movement of molecular chains and finally achieving the effects of increasing the fluidity and toughening of the material.
In some embodiments, the degradable glass fiber comprises: siO 2 70-80wt％;Al2O3 2-4wt％;Na2O15-19wt％;K2 O1-3wt%; 5-15wt% of CaO and/or MgO; the heat-resistant modification auxiliary agent is an aromatic sulfonate derivative, and is preferably a crystallization nucleating agent LAK301. In the embodiment of the invention, although the glass fiber can be used as the nucleating agent of the biodegradable resin polylactic acid material, the nucleating effect and the nucleating rate are insufficient, so that the crystallization nucleating agent LAK301 is introduced as a heat-resistant modification auxiliary agent in the embodiment of the invention, and the glass fiber and the crystallization nucleating agent are simultaneously used as the nucleating agent to promote the crystallization nucleating effect of the composite material. Meanwhile, the glass fiber belongs to a rigid material and can play a supporting role when the biodegradable resin polylactic acid is softened by heating, so that the heat resistance of the composite material is increased by the crystallization of the biodegradable resin polylactic acid, and the heat resistance of the composite material is increased by the rigidity of the glass fiber.
In some embodiments, the inorganic filler material comprises at least one of talc, calcium carbonate, montmorillonite; the lubricant comprises at least one of erucamide, oleamide and wax substances. According to the embodiment of the invention, the inorganic filler is added, so that the material cost can be reduced, the lubricant is added, the product can be smoothly demoulded, the screw torque is reduced, and the energy consumption is saved.
The embodiment of the invention also provides a preparation method of the degradable composite material for thin-wall injection molding, which comprises the following steps:
a. Pretreatment of degradable glass fibers: firstly, putting the degradable glass fiber and the fiber surface treating agent into a mixer together, and fully mixing, wherein the temperature of the mixer is preferably controlled to be 60-80 ℃;
b. Mixing biodegradable resin, a toughening agent, a flow promoter, a compatilizer, an inorganic filling material, a heat-resistant modification auxiliary agent and a lubricant according to a designed proportion, adding the mixture into a double-screw extruder, adding the glass fiber pretreated in the step a in a side feeding mode, and carrying out co-extrusion granulation in the double-screw extruder, wherein the extrusion temperature is preferably 150-190 ℃, so as to obtain the degradable composite material.
The preparation method of the degradable composite material for thin-wall injection molding provided by the embodiment of the invention has the advantages that the process is simple, the processing can be directly completed by adopting common equipment, the industrial application is easy, the prepared composite material has good fluidity and excellent temperature resistance and mechanical property, and the requirements of thin-wall injection molding products can be met. In the method of the embodiment of the invention, as the shape of the glass fiber and the shape of other materials are greatly different, if the glass fiber and the other materials are mixed together, the fiber bundles are dispersed so as to be difficult to discharge.
The present invention will be described in detail with reference to examples.
Example 1
(1) Glass fiber pretreatment
Adding 20 parts by weight of degradable glass fibers and 2 parts by weight of PEG400 into a high-speed mixer, controlling the mixing temperature to be 70 ℃, and fully mixing to obtain pretreated degradable glass fibers;
(2) Preparation of composite materials
50 Parts by weight of polylactic acid (with the weight-average molecular weight of 20 ten thousand), 10 parts by weight of polybutylene succinate, 5 parts by weight of low-molecular-weight polylactic acid (with the molecular weight of 4000), 2 parts by weight of polyethylene glycol/lactic acid copolymer, 10 parts by weight of talcum powder, 0.5 part by weight of nucleating agent LAK301 and 0.5 part by weight of erucic acid amide are mixed, added into a double-screw extruder, and the pretreated glass fiber is added through side feeding of the double-screw extruder to carry out mixed extrusion granulation, wherein the extrusion process parameters are as follows: the temperature is 140-180 ℃, the rotation speed of a host machine is 260rpm, and the feeding rotation speed is 65rpm, so that the degradable composite material is prepared.
The components of the degradable composite material prepared in the embodiment are shown in table 1, and the performance data are shown in table 2.
Example 2
(1) Glass fiber pretreatment
Adding 20 parts by weight of degradable glass fibers and 1 part by weight of PEG400 into a high-speed mixer, controlling the mixing temperature to be 60 ℃, and fully mixing to obtain pretreated degradable glass fibers;
(2) Preparation of composite materials
53 Parts by weight of polylactic acid (weight average molecular weight is 10 ten thousand), 5 parts by weight of polybutylene succinate, 5 parts by weight of poly (succinic acid) -adipic acid-butanediol ester, 3 parts by weight of low molecular weight polylactic acid (molecular weight is 6000), 2 parts by weight of polyethylene glycol/lactic acid copolymer, 10 parts by weight of talcum powder, 0.5 part by weight of nucleating agent LAK301 and 0.5 part by weight of erucamide are mixed, added into a double-screw extruder, and the pretreated glass fiber is added through side feeding of the double-screw extruder to carry out mixed extrusion granulation, wherein the extrusion process parameters are as follows: the temperature is 140-180 ℃, the rotation speed of a host machine is 260rpm, and the feeding rotation speed is 65rpm, so that the degradable composite material is prepared.
The components of the degradable composite material prepared in the embodiment are shown in table 1, and the performance data are shown in table 2.
Example 3
(1) Glass fiber pretreatment
Adding 20 parts by weight of degradable glass fibers and 1 part by weight of PEG400 into a high-speed mixer, controlling the mixing temperature to be 60 ℃, and fully mixing to obtain pretreated degradable glass fibers;
(2) Preparation of composite materials
50 Parts by weight of polylactic acid (weight average molecular weight is 10 ten thousand), 15 parts by weight of poly succinic acid-adipic acid-butanediol ester, 1 part by weight of low molecular weight polylactic acid (molecular weight is 2000), 2 parts by weight of polyethylene glycol/lactic acid copolymer, 10 parts by weight of talcum powder, 0.5 part by weight of nucleating agent LAK301 and 0.5 part by weight of erucamide are mixed, added into a double-screw extruder, and the pretreated glass fiber is added through side feeding of the double-screw extruder to carry out mixed extrusion granulation, wherein the extrusion process parameters are as follows: the temperature is 140-180 ℃, the rotation speed of a host machine is 260rpm, and the feeding rotation speed is 65rpm, so that the degradable composite material is prepared.
The components of the degradable composite material prepared in the embodiment are shown in table 1, and the performance data are shown in table 2.
Example 4
The same procedure as in example 1 was followed except that the content of the components was varied.
The components of the degradable composite material prepared in the embodiment are shown in table 1, and the performance data are shown in table 2.
Comparative example 1
The same procedure as in example 1 was followed except that the glass fibers were not pretreated with PEG400, but instead, the glass fiber material was directly fed into a twin screw extruder via a side feed, and extrusion pelletization was performed by mixing with the other raw materials.
The degradable composite material prepared in comparative example 1 has the components shown in table 1 and the performance data shown in table 2.
Comparative example 2
The same procedure as in example 1 was followed except that the polyethylene glycol/lactic acid copolymer was not added.
The components of the degradable composite material prepared in comparative example 2 are shown in table 1, and the performance data are shown in table 2.
Comparative example 3
The same procedure as in example 1 was followed except that low molecular weight polylactic acid was not added.
The components of the degradable composite material prepared in the comparative example 3 are shown in table 1, and the performance data are shown in table 2.
Comparative example 4
The same procedure as in example 1 was followed except that no nucleating agent LAK301 was added.
The degradable composite material prepared in comparative example 4 has the components shown in table 1 and the performance data shown in table 2.
Comparative example 5
The same procedure as in example 1 was followed except that low molecular weight polylactic acid and polyethylene glycol/lactic acid copolymer were not added, and that the glass fiber was not pretreated with PEG400, but the glass fiber material was directly fed into a twin screw extruder via a side feed, and was mixed with other raw materials for extrusion granulation.
The degradable composite material prepared in comparative example 5 has the components shown in table 1 and the performance data shown in table 2.
Comparative example 6
The same procedure as in example 1 was followed except that low molecular weight polylactic acid, polyethylene glycol/lactic acid copolymer and nucleating agent LAK301 were not added, and that the glass fiber was not pretreated with PEG400, but the glass fiber material was directly fed into a twin screw extruder via a side feed and mixed with the other raw materials for extrusion granulation.
The degradable composite material prepared in comparative example 6 has the components shown in table 1 and the performance data shown in table 2.
TABLE 1
TABLE 2
Note that: 1. the tensile strength and elongation at break test standard is GB/T1040;
2. The bending strength test standard is GB/T9341;
3. The thermal deformation temperature test standard is GB/T1634;
4. The melt flow rate test standard was GB/T3682.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (6)
1. A degradable composite material for thin-wall injection molding, comprising: 30-80 parts of biodegradable resin, 10-50 parts of toughening agent, 1-5 parts of flow promoter, 5-20 parts of degradable glass fiber, 1-5 parts of fiber surface treatment agent, 1-5 parts of compatilizer, 5-20 parts of inorganic filling material, 0.2-1 part of heat-resistant modification auxiliary agent and 0.1-0.8 part of lubricant by mass, wherein the biodegradable resin comprises polylactic acid, and the weight average molecular weight of the biodegradable resin is 8-30 ten thousand;
The flow promoter is low-molecular-weight polylactic acid, and the molecular weight of the flow promoter is 2000-8000;
the fiber surface treating agent is polyethylene glycol;
The compatilizer is polyethylene glycol/lactic acid copolymer;
the melt flow rate of the degradable composite material for thin-wall injection molding is 60-120 g/10min;
the preparation method of the degradable composite material for thin-wall injection molding comprises the following steps:
a. pretreatment of degradable glass fibers: firstly, putting degradable glass fiber and a fiber surface treating agent together in a mixer, and fully mixing;
b. And d, mixing the biodegradable resin, the toughening agent, the flow promoter, the compatilizer, the inorganic filling material, the heat-resistant modification auxiliary agent and the lubricant according to a designed proportion, adding the mixture into a double-screw extruder, adding the glass fiber pretreated in the step a in a side feeding mode, and carrying out co-extrusion granulation in the double-screw extruder to obtain the degradable composite material.
2. The degradable composite material for thin-wall injection molding according to claim 1, wherein the toughening agent is a flexible biodegradable resin comprising at least one of polybutylene succinate and polybutylene succinate-adipic acid-butylene succinate.
3. The degradable composite for thin-wall injection molding of claim 1, wherein the degradable glass fiber comprises:
SiO270-80wt%；
Al2O3 2-4wt%；
Na2O15-19wt%；
K2O1-3wt%；
CaO and/or MgO5-15wt%
The sum of the contents of the components is 100 percent.
4. The degradable composite material for thin-wall injection molding according to claim 1, wherein the inorganic filler comprises at least one of talc powder, calcium carbonate, montmorillonite; the lubricant comprises at least one of erucamide, oleamide and wax substances.
5. The degradable composite material for thin-wall injection molding according to claim 1, wherein the heat-resistant modifying aid is an aromatic sulfonate derivative.
6. The degradable composite material for thin-wall injection molding according to claim 1, wherein in the step a, the temperature of the mixer is controlled to be 60-80 ℃; in the step b, the extrusion temperature is 150-190 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087488A (en) * | 2013-01-31 | 2013-05-08 | 金发科技股份有限公司 | Biodegradable polylactic acid composite material, and preparation method and application thereof |
| CN103665800A (en) * | 2012-09-18 | 2014-03-26 | 上海载和实业投资有限公司 | Continuous fiber reinforced polylactic resin composition and preparation method thereof |
| CN113845761A (en) * | 2021-08-18 | 2021-12-28 | 浙江中科应化生态新材料科技有限公司 | High-transparency completely degradable film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103665800A (en) * | 2012-09-18 | 2014-03-26 | 上海载和实业投资有限公司 | Continuous fiber reinforced polylactic resin composition and preparation method thereof |
| CN103087488A (en) * | 2013-01-31 | 2013-05-08 | 金发科技股份有限公司 | Biodegradable polylactic acid composite material, and preparation method and application thereof |
| CN113845761A (en) * | 2021-08-18 | 2021-12-28 | 浙江中科应化生态新材料科技有限公司 | High-transparency completely degradable film and preparation method thereof |
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