CN115678221B - Full-biodegradable bone strip material and preparation method thereof - Google Patents

Full-biodegradable bone strip material and preparation method thereof Download PDF

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CN115678221B
CN115678221B CN202211450312.3A CN202211450312A CN115678221B CN 115678221 B CN115678221 B CN 115678221B CN 202211450312 A CN202211450312 A CN 202211450312A CN 115678221 B CN115678221 B CN 115678221B
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mixing
calcium carbonate
bone strip
diatomite
superfine
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CN115678221A (en
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秦超
朱文君
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Anhui Buchao Environmental Protection Technology Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W90/00Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
    • Y02W90/10Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics

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Abstract

The invention provides a full-biodegradable bone strip material and a preparation method thereof, and relates to the technical field of full-biodegradable material processing. The fully biodegradable bone strip material is prepared from modified polylactic acid, PBAT, nano calcium carbonate, superfine calcium carbonate, modified plant fiber, superfine starch, diatomite, a plasticizer, a coupling agent and an opening agent through the steps of mixing and freeze-drying the modified plant fiber, the superfine calcium carbonate and the superfine starch, calcining the diatomite to adsorb the nano calcium carbonate, centrifuging and drying, and mixing and extruding the raw materials. The invention overcomes the defects of the prior art, effectively ensures the degradation efficiency of the fully degraded material, and improves the toughness of the material, so that the bone strip manufactured by the material can be bent, opened and used for a plurality of times, and simultaneously ensures the tightness of the whole material when in use, and improves the environmental protection of the production and use of the sealing bag.

Description

Full-biodegradable bone strip material and preparation method thereof
Technical Field
The invention relates to the technical field of processing of fully biodegradable materials, in particular to a fully biodegradable bone strip material and a preparation method thereof.
Background
The full-biodegradable material is a material which can be completely decomposed into low-molecular compounds by microorganisms (such as bacteria, fungi, algae and the like) under proper and natural environment conditions capable of indicating the term, and the full-biodegradable material gradually starts to replace the traditional plastic along with development of technology and importance of people on environmental protection so as to effectively solve the problem of white pollution.
In the prior art, most of the fully degradable materials are prepared into disposable daily appliances such as films, convenience bags, disposable tableware and the like, wherein the convenience bags are most common, a large number of plastic bags are consumed in society each year before the fully degradable materials, and because of the characteristic of difficult degradation, the fully degradable materials bring a large burden to the environment, and correspondingly, in order to improve the environmental protection, a plurality of places start to go out of a platform to limit plastic, so that the use of the plastic bags and the disposable tableware is reduced, namely the fully degradable biological materials are widely applied on the basis.
The fully biodegradable material has the properties of water resistance, portability and the like similar to plastics, can be widely used for replacing the traditional plastic materials, particularly the disposable packaging material, can effectively reduce the pollution of the plastics by adopting the fully biodegradable material, and has more and more products for replacing the plastics with the fully biodegradable material along with the market demands.
The sealing bag is a packaging bag which is commonly used for preserving and sealing food or articles in daily life, and can conveniently seal and store the articles along with the development of fully degradable materials, the bag body of the sealing bag can be replaced by the fully degradable materials, but the sealing bone strip is inevitably folded in the using process due to the continuous opening and closing of the sealing bone strip, and the sealing bone strip is seriously affected by the damage caused by the difference between the toughness of the sealing bone strip and the common plastic after the sealing bone strip is folded and repeatedly opened and used, so that most of the degradable sealing bags are generally prepared from the fully degradable materials at the present stage, and the sealing bone strip is prepared from the traditional PE or PVC materials so as to ensure the using tightness of the whole sealing bag.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the full-biodegradable bone strip material and the preparation method thereof, which effectively ensure the degradation efficiency of the full-degradable material, and simultaneously improve the toughness of the material, so that the bone strip prepared by the material can be bent, opened and used for a plurality of times, and simultaneously ensure the tightness of the whole material in use, and improve the environmental protection of the production and use of the sealing bag.
In order to achieve the above object, the technical scheme of the present invention is realized by the following technical scheme:
the full-biodegradable bone strip material is prepared from the following raw materials in parts by weight: 12-15 parts of modified polylactic acid, 35-50 parts of PBAT, 4-6 parts of nano calcium carbonate, 14-20 parts of superfine calcium carbonate, 10-12 parts of modified plant fiber, 10-12 parts of superfine starch, 4-6 parts of diatomite, 0.8-1.4 parts of plasticizer, 0.5-0.8 part of coupling agent and 0.4-0.6 part of opening agent.
Preferably, the particle size of the nano calcium carbonate is 10-100nm, the particle size of the superfine calcium carbonate is 0.3-4 mu m, and the particle size of the superfine starch is 0.1-3 mu m.
Preferably, the modified polylactic acid is obtained by blending modified nano cellulose surface silane with polylactic acid.
Preferably, the plasticizer is any one or more of glycerol, ethylene glycol, sorbitol and polyvinyl alcohol.
Preferably, the modified plant fiber is prepared by soaking kenaf fiber in an acidic solution with pH of 6.5 for 30min, taking out, washing, and drying to obtain the modified plant fiber.
The preparation method of the full-biodegradable bone strip comprises the following steps:
(1) Pretreatment of raw materials: dispersing superfine calcium carbonate in clear water, adding modified plant fibers, performing ultrasonic oscillation, adding superfine starch into the mixture, uniformly stirring the mixture in a water bath, and freeze-drying and crushing the mixture to obtain a pretreated material for later use;
(2) Diatomite pretreatment: roasting diatomite at 500 ℃ for 2 hours, taking out, putting the diatomite into 75% ethanol solution, mixing with nano calcium carbonate, centrifuging, and drying the centrifugal precipitate to obtain pretreated diatomite for later use;
(3) And (3) mixing: mixing the pretreated material, pretreated diatomite, modified polylactic acid, PBAT, plasticizer, coupling agent and opening agent in a mixer to obtain a mixture for standby;
(4) And (3) forming: and (3) putting the mixture into a double-screw granulator, mixing and granulating, cooling the granules, and putting the cooled granules into a bone strip machine for molding to obtain the full-biological degradable bone strip.
Preferably, the temperature of the water bath stirring in the step (1) is 60-65 ℃, the stirring rotating speed is 120-150r/min, and the stirring time is 15-20min.
Preferably, the rotational speed of the centrifugation in the step (2) is 4200r/min, and the centrifugation time is 10min.
Preferably, the rotational speed of the mixing in the mixer in the step (3) is 600-800r/min, and the mixing time is 20-30min.
Preferably, the process of the double-screw extrusion granulation in the step (4) is that the double-screw extruder is used for mixing in a first zone for 20-30min, a second zone for 40-50min, a third zone for 15-20min and a fourth zone for 40-50min, the temperatures of the first zone and the second zone are 165 ℃, and the temperatures of the third zone and the fourth zone are 160 ℃.
The invention provides a full-biodegradable bone strip material and a preparation method thereof, which have the advantages compared with the prior art that:
(1) According to the invention, calcium carbonate is added into the fully degradable material, the calcium carbonate can increase the distance between resin molecules, reduce the acting force of a high molecular chain segment, block the re-crosslinking of macromolecular free radicals and accelerate the degradation of biodegradable plastics, and meanwhile, the calcium carbonate with different particle diameters is added in an auxiliary way and mixed with modified plant fibers, so that the skeleton structure of the whole material can be effectively ensured, the toughness of the prepared bone strip material is ensured, the deformation is effectively prevented, and the tightness of the subsequent bone strip is improved.
(2) The plant fiber is provided with more pores through acid treatment, is mixed with superfine calcium carbonate and then freeze-dried, the superfine calcium carbonate is adsorbed in the pores of the plant fiber to form a stable skeleton structure, superfine starch is mixed in a water bath to enable the superfine starch to be semi-gelatinized to wrap the plant fiber, then the plant fiber is dried and crushed, more pore structures exist outside the starch wrapping to facilitate the mixing with the subsequent raw materials, and meanwhile, the toughness of the whole material is improved, and the degradation effect of the material is ensured;
(3) According to the invention, the diatomite is calcined to adsorb nano calcium carbonate to form a stable compact framework, and then the stable compact framework is mixed with the rest raw materials, so that the integral deformation resistance of the material is effectively improved, the toughness of the material is ensured, the material is prevented from being deformed under multiple bending, the material is ensured to have good tightness after being repeatedly opened and closed after being prepared into the bone strip, the replacement of the material to the traditional plastic bone strip is improved, and the effect of environmental friendliness is achieved.
Description of the drawings:
FIG. 1 is a schematic diagram of a bone strip made from bone strip material according to example 3 of the present invention;
fig. 2 is a schematic diagram of sealing a bone strip prepared from bone strip material in a sealing bag according to embodiment 3 of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
preparation of raw materials:
preparation of modified polylactic acid: mixing nano cellulose with KH-550 for modification, taking out and drying to obtain surface modified nano cellulose, and blending polylactic acid and the surface modified nano cellulose according to the mass ratio of 100:2 to obtain modified polylactic acid;
modified plant fiber: soaking kenaf fiber in an acidic solution with pH of 6.5 for 30min, taking out, washing, and drying to obtain modified plant fiber;
nano calcium carbonate: selecting calcium carbonate particles with the particle size within the range of 10-100nm as nano calcium carbonate;
superfine calcium carbonate: selecting calcium carbonate particles with the particle size of 0.3-4 mu m as nano calcium carbonate;
superfine starch: selecting starch particles with the particle size of 0.3-4 mu m as superfine starch;
example 2:
preparation of fully biodegradable bone stock (using the raw materials obtained in example 1 above):
(1) Dispersing 7kg of superfine calcium carbonate in clear water, adding 5kg of modified plant fiber, performing ultrasonic vibration for 5min, adding 5kg of superfine starch, uniformly stirring at a water bath temperature of 60 ℃ at a stirring speed of 120r/min for 15min, freeze-drying at a temperature of minus 15 ℃ and crushing to obtain a pretreated material for later use;
(2) Roasting 2kg of diatomite at 500 ℃ for 2 hours, taking out, placing the diatomite in 75% ethanol solution, mixing with 2kg of nano calcium carbonate, centrifuging for 10 minutes at a rotating speed of 4200r/min, and drying the centrifugal precipitate to obtain pretreated diatomite for later use;
(3) Mixing the pretreated material, pretreated diatomite, 6kg of modified polylactic acid, 17.5kg of PBAT, 0.4kg of ethylene glycol, 0.25kg of JS-A151 silane coupling agent and 0.2kg of opening agent in a mixer for 20min at the rotating speed of 600r/min to obtain a mixture for standby;
(4) Placing the mixture into a double-screw granulator, regulating the temperature of a first region and a second region to 165 ℃, regulating the temperature of a third region and a fourth region to 160 ℃, mixing for 20min in the first region, mixing for 50min in the second region, mixing for 15min in the third region, mixing for 50min in the fourth region, extruding and granulating, and obtaining the full-biodegradable bone strip.
Example 3:
preparation of fully biodegradable bone stock (using the raw materials obtained in example 1 above):
(1) Dispersing 10kg of superfine calcium carbonate in clear water, adding 6kg of modified plant fibers, carrying out ultrasonic oscillation for 5min, adding 6kg of superfine starch, uniformly stirring at a stirring speed of 150r/min for 20min at a water bath temperature of 65 ℃, freeze-drying at a temperature of minus 15 ℃ and crushing to obtain a pretreated material for later use;
(2) Roasting 3kg of diatomite at 500 ℃ for 2 hours, taking out, placing the diatomite in 75% ethanol solution, mixing with 3kg of nano calcium carbonate, centrifuging for 10 minutes at a rotating speed of 4200r/min, and drying the centrifugal precipitate to obtain pretreated diatomite for later use;
(3) Mixing the pretreated material, pretreated diatomite, 7.5kg of modified polylactic acid, 25kg of PBAT, 0.7kg of ethylene glycol, 0.4kg of JS-A151 silane coupling agent and 0.3kg of opening agent in a mixer for 30min at the rotating speed of 800r/min to obtain a mixture for standby;
(4) Placing the mixture into a double-screw granulator, regulating the temperature of a first region and a second region to 165 ℃, regulating the temperature of a third region and a fourth region to 160 ℃, mixing for 30min in the first region, mixing for 40min in the second region, mixing for 20min in the third region, mixing for 40min in the fourth region, extruding and granulating to obtain the full-biodegradable bone strip.
Comparative example 1:
preparation of fully biodegradable bone stock (using the raw materials obtained in example 1 above):
(1) Dispersing 10kg of superfine calcium carbonate in clear water, adding 6kg of modified plant fibers, carrying out ultrasonic oscillation for 5min, adding 6kg of superfine starch, uniformly stirring at a stirring speed of 150r/min for 20min at a water bath temperature of 65 ℃, freeze-drying at a temperature of minus 15 ℃ and crushing to obtain a pretreated material for later use;
(2) Roasting 3kg of diatomite at 500 ℃ for 2 hours, taking out, placing the diatomite in 75% ethanol solution, mixing with 3kg of nano calcium carbonate, centrifuging for 10 minutes at a rotating speed of 4200r/min, and drying the centrifugal precipitate to obtain pretreated diatomite for later use;
(3) Mixing the pretreated material, pretreated diatomite, 7.5kg of polylactic acid, 25kg of PBAT, 0.7kg of glycol, 0.4kg of JS-A151 silane coupling agent and 0.3kg of opening agent in a mixer for 30min at the rotating speed of 800r/min to obtain a mixture for standby;
(4) Placing the mixture into a double-screw granulator, regulating the temperature of a first region and a second region to 165 ℃, regulating the temperature of a third region and a fourth region to 160 ℃, mixing for 30min in the first region, mixing for 40min in the second region, mixing for 20min in the third region, mixing for 40min in the fourth region, extruding and granulating to obtain the full-biodegradable bone strip.
Comparative example 2:
preparation of fully biodegradable bone stock (using the raw materials obtained in example 1 above):
(1) 10kg of superfine calcium carbonate, 6kg of modified plant fibers, 6kg of superfine starch, 3kg of diatomite, 3kg of nano calcium carbonate, 7.5kg of polylactic acid, 25kg of PBAT, 0.7kg of ethylene glycol, 0.4kg of JS-A151 silane coupling agent and 0.3kg of opening agent are mixed in a mixer for 30min at the rotating speed of 800r/min, so as to obtain a mixture for standby;
(2) Placing the mixture into a double-screw granulator, regulating the temperature of a first region and a second region to 165 ℃, regulating the temperature of a third region and a fourth region to 160 ℃, mixing for 30min in the first region, mixing for 40min in the second region, mixing for 20min in the third region, mixing for 40min in the fourth region, extruding and granulating to obtain the full-biodegradable bone strip.
And (3) detection:
1. the degradation effect of the fully biodegradable bone chips obtained in the examples 2-3 and comparative examples 1-2 on the market was examined, and a thin-layer chromatographic grade cellulose was used as a reference material: the biological decomposition rate was measured by using GB/T19277.1-2011 standard, and the results are shown in Table 1 below:
TABLE 1
As can be seen from Table 1 above, the bone fragments prepared in examples 2-3 had a higher biological decomposition rate at 122d than the materials prepared in comparative examples 1-2.
2. The mechanical properties of the bone fragments prepared in examples 2 to 3 and comparative examples 1 to 2 were measured, and the water vapor barrier properties and water repellency of each group of materials were measured with reference to GB/T26153-2010 and GB/T19789-2005, respectively, as shown in Table 2 below:
TABLE 2
Group of Example 2 Example 3 Comparative example 1 Comparative example 2
Tensile Strength (MPa) 43.9 45.1 34.9 36.6
Elongation at break (%) 309.2 311.4 229.7 235.6
Water vapor transmission rate (gm. R) -2 ·d -1 ) 1.7 1.6 2.6 2.3
Oxygen permeability (ml.m) -2 ·d -1 ) 1.4 1.4 2.1 1.9
As is clear from Table 2 above, the bone chips prepared in examples 2-3 had good mechanical properties and excellent sealability.
3. Molding the bone strip materials prepared in the examples 2-3 and the comparative examples 1-2 in a bone strip machine to obtain a full-biodegradable bone strip; bending and opening the bone strips obtained in each group, namely mounting the bone strips obtained in each group at the opening of the sealing bag, bending left and right for 60-70 degrees after closing, bending for 500 times in total, recording the deformation condition of the bone strips, opening and closing the bone strips mounted at the opening of the sealing bag for 500 times, closing the bone strips again, detecting whether the sealing position of the bone strips of the sealing bag leaks or not after closing, and recording the following table 3:
TABLE 3 Table 3
As can be seen from Table 3 above, the bone fragments prepared in examples 2-3 still maintain good shape after multiple bending, and are not easily deformed.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims (7)

1. The preparation method of the fully biodegradable bone strip material is characterized by comprising the following steps of:
(1) Pretreatment of raw materials: dispersing superfine calcium carbonate in clear water, adding modified plant fibers, performing ultrasonic oscillation, adding superfine starch into the mixture, uniformly stirring the mixture in a water bath, and freeze-drying and crushing the mixture to obtain a pretreated material for later use;
(2) Diatomite pretreatment: roasting diatomite at 500 ℃ for 2 hours, taking out, putting the diatomite into 75% ethanol solution, mixing with nano calcium carbonate, centrifuging, and drying the centrifugal precipitate to obtain pretreated diatomite for later use;
(3) And (3) mixing: mixing the pretreated material, pretreated diatomite, modified polylactic acid, PBAT, plasticizer, coupling agent and opening agent in a mixer to obtain a mixture for standby;
(4) And (3) forming: putting the mixture into a double-screw granulator, carrying out mixed granulation, cooling the granules, and then putting the cooled granules into a bone strip machine for molding to obtain full-biological degradable bone strips;
the total biodegradable bone strip comprises the following raw materials in parts by weight: 12-15 parts of modified polylactic acid, 35-50 parts of PBAT, 4-6 parts of nano calcium carbonate, 14-20 parts of superfine calcium carbonate, 10-12 parts of modified plant fiber, 10-12 parts of superfine starch, 4-6 parts of diatomite, 0.8-1.4 parts of plasticizer, 0.5-0.8 part of coupling agent and 0.4-0.6 part of opening agent;
the modified polylactic acid is obtained by blending modified nano cellulose surface silane with polylactic acid; the preparation method of the modified plant fiber comprises the steps of soaking kenaf fiber in an acidic solution with the pH of 6.5 for 30min, taking out, washing, and drying to obtain the modified plant fiber.
2. The method for preparing the fully biodegradable bone strip according to claim 1, wherein the method comprises the following steps: the particle size of the nano calcium carbonate is 10-100nm, the particle size of the superfine calcium carbonate is 0.3-4 mu m, and the particle size of the superfine starch is 0.1-3 mu m.
3. The method for preparing the fully biodegradable bone strip according to claim 1, wherein the method comprises the following steps: the plasticizer is any one or more of glycerol, ethylene glycol, sorbitol and polyvinyl alcohol.
4. The method for preparing the fully biodegradable bone strip according to claim 1, wherein the method comprises the following steps: the temperature of the water bath stirring in the step (1) is 60-65 ℃, the stirring rotating speed is 120-150r/min, and the stirring time is 15-20min.
5. The method for preparing the fully biodegradable bone strip according to claim 1, wherein the method comprises the following steps: the rotational speed of centrifugation in the step (2) is 4200r/min, and the centrifugation time is 10min.
6. The method for preparing the fully biodegradable bone strip according to claim 1, wherein the method comprises the following steps: the rotational speed of mixing in the mixer in the step (3) is 600-800r/min, and the mixing time is 20-30min.
7. The method for preparing the fully biodegradable bone strip according to claim 1, wherein the method comprises the following steps: the process of double-screw extrusion granulation in the step (4) comprises mixing in a first zone for 20-30min, mixing in a second zone for 40-50min, mixing in a third zone for 15-20min and mixing in a fourth zone for 40-50min in a double-screw extruder, wherein the temperatures of the first zone and the second zone are 165 ℃, and the temperatures of the third zone and the fourth zone are 160 ℃.
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CN112876745A (en) * 2021-02-04 2021-06-01 杭州之西科技有限公司 Antibacterial biodegradable tableware and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN109081955A (en) * 2018-07-02 2018-12-25 界首市汇珠渔具有限公司 A kind of starch-based bio degradable bionic fish bait adding modified nano calcium carbonate
CN109486139A (en) * 2018-11-14 2019-03-19 江苏省农业科学院 Environment-friendly toughened nano-cellulose-polylactic acid biodegradation material and preparation method thereof
CN112876745A (en) * 2021-02-04 2021-06-01 杭州之西科技有限公司 Antibacterial biodegradable tableware and preparation method thereof

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