CN112745647A - Non-breathable biodegradable resin and preparation method thereof - Google Patents
Non-breathable biodegradable resin and preparation method thereof Download PDFInfo
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- CN112745647A CN112745647A CN202011623134.0A CN202011623134A CN112745647A CN 112745647 A CN112745647 A CN 112745647A CN 202011623134 A CN202011623134 A CN 202011623134A CN 112745647 A CN112745647 A CN 112745647A
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- biodegradable resin
- screw extrusion
- breathable biodegradable
- titanium dioxide
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- 229920006167 biodegradable resin Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 26
- 238000001125 extrusion Methods 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 229920001896 polybutyrate Polymers 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000010008 shearing Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 12
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 10
- 239000000600 sorbitol Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- 238000005507 spraying Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 238000004806 packaging method and process Methods 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 3
- 229920000747 poly(lactic acid) Polymers 0.000 description 3
- 239000004626 polylactic acid Substances 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- PTIXVVCRANICNC-UHFFFAOYSA-N butane-1,1-diol;hexanedioic acid Chemical compound CCCC(O)O.OC(=O)CCCCC(O)=O PTIXVVCRANICNC-UHFFFAOYSA-N 0.000 description 2
- JYLRDAXYHVFRPW-UHFFFAOYSA-N butane-1,1-diol;terephthalic acid Chemical compound CCCC(O)O.OC(=O)C1=CC=C(C(O)=O)C=C1 JYLRDAXYHVFRPW-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010096 film blowing Methods 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Abstract
The invention provides a non-breathable biodegradable resin and a preparation method thereof, wherein the preparation method comprises the following steps: s1, mixing PLA and PBAT according to the mass ratio of 5-9: 1-3, drying, and spraying a sorbitol solution accounting for 3-7% of the weight of the blend on the surface of the mixture after drying; s2, carrying out screw extrusion treatment on the product obtained in the step S1; s3, blending the product obtained in the step S2 and titanium dioxide accounting for 6-9% of the weight of the product, and carrying out high-speed shearing treatment on the blend by using a high-speed shearing machine; and S4, carrying out screw extrusion treatment on the obtained substance in the S3, then bracing, cooling and finally cutting to obtain the non-breathable biodegradable resin. The invention adopts a two-stage blending process, so that the materials are more fully mixed and better dispersed, and the problems of large bubble vibration and inconsistent color degree outside the film are solved; the obtained resin has the advantages of high tensile strength, high elongation at break, biodegradability and the like, and can be widely applied to preparation of food packaging, medical care, medical protective tools and the like.
Description
Technical Field
The invention relates to the technical field of biodegradable resin and a preparation method thereof, in particular to non-breathable biodegradable resin.
Background
The biodegradable resin has the advantages of biodegradation and wide application prospect. In the preparation raw materials of the biodegradable resin, PLA (polylactic acid) has good biodegradability, can be completely degraded by microorganisms in the nature under specific conditions after being used, finally generates carbon dioxide and water, does not pollute the environment, and is a well-known environment-friendly material;
PBAT is a copolymer of butanediol adipate and butanediol terephthalate, has the characteristics of PBA (butanediol adipate) and PBT (butanediol terephthalate), and has better ductility and elongation at break as well as better heat resistance and impact performance; it has excellent biodegradability, and is one of the best degradable materials in the market.
PLA and PBAT belong to aliphatic resin, but the compatibility of the two materials is poor, and due to the influence of the process in the prior art, the dispersion is insufficient, the membrane bubble jitter is large, the color degree outside the membrane is inconsistent (the outside is bright) in the production process, and the quality requirement of the non-breathable biodegradable resin cannot be met.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation method of non-breathable biodegradable resin, which solves the problem that the quality of the non-breathable biodegradable resin does not reach the standard due to the preparation process in the prior art.
According to an embodiment of the invention, a method for preparing a non-breathable biodegradable resin comprises the following steps:
s1, mixing PLA and PBAT according to the mass ratio of 5-9: 1-3, drying, and spraying a sorbitol solution accounting for 3-7% of the weight of the blend on the surface of the mixture after drying;
s2, carrying out screw extrusion treatment on the product obtained in the step S1;
s3, blending the product obtained in the step S2 and titanium dioxide accounting for 6-9% of the weight of the product, and carrying out high-speed shearing treatment on the blend by using a high-speed shearing machine;
and S4, carrying out screw extrusion treatment on the obtained substance in the S3, then bracing, cooling and finally cutting to obtain the non-breathable biodegradable resin.
Furthermore, the solvent of the sorbitol solution is pure water, the mass concentration of the pure water is 40-60%, and the sorbitol is in a food additive grade, so that the sorbitol solution is a chain extender with high safety.
Further, PLA and PBAT in S1 are soaked in 75-95% ethanol for 3' 5h and then dried, wherein the drying temperature is 60-70 ℃, and the drying time is 2-3 h. The used PLA and PBAT are granular and can separate out a small amount of impurities contained in the granules after being soaked in ethanol.
Further, the screw extrusion in S2 is twin-screw extrusion, the temperature is 150-170 ℃, the screw rotation speed is 360-.
Further, when blending in S3 and S3, titanium dioxide is divided into four parts of 15%, 25%, 25% and 35% by weight and added into the product obtained in S2 for four times.
Furthermore, the time interval for adding the titanium dioxide in portions is 0.5-1 min, and stirring is continuously carried out at 50-100 r/min in the adding process.
Further, the stirring in the process of adding the titanium dioxide is magnetic stirring.
Further, the high-speed shearing process in S3 is in the following two stages:
the first stage is as follows: treating for 20-30 min at 300-500 r/min;
the second stage is 8000-12000 r/min for 10-15 min. The first stage is carried out low-speed stirring, so that the added titanium dioxide solution is quickly distributed to each position of the high-speed shearing machine and is simultaneously contained in PLA and PBAT, and in the second stage, high-speed shearing is carried out, so that the blending of the titanium dioxide, the PLA and the PBAT is realized, the titanium dioxide is fully dispersed in the blend,
further, the screw extrusion in S4 is twin-screw extrusion, the temperature is 120-140 ℃, the screw rotation speed is 300-350r/min, and the mold stripping pressure is 3-5 MPa.
According to the embodiment of the invention, the non-breathable biodegradable resin prepared by the process is also provided.
Compared with the prior art, the invention has the following beneficial effects:
by adopting a two-stage blending process (namely, carrying out double-screw extrusion treatment twice), the materials are more fully mixed and better dispersed, and the problems of large bubble vibration and inconsistent external color of the film are solved;
the obtained resin has the advantages of high tensile strength, high elongation at break, biodegradability and the like, and the used raw and auxiliary materials have high safety and can be widely applied to the preparation of food packaging, medical care, medical protective appliances and the like.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples.
Example 1
The embodiment provides a preparation method of a non-breathable biodegradable resin, which comprises the following steps:
s1, mixing PLA and PBAT according to the proportion of 500g:100g, drying at 60 ℃ for 3h, and spraying a sorbitol aqueous solution with the mass concentration of 40% accounting for 7% of the weight of the blend on the surface of the blend after drying;
s2, extruding the product obtained in the step S1 by a double screw at the temperature of 150 ℃, the rotating speed of the screw is 380r/min, and the mold stripping pressure is 8 Mpa;
s3, blending the obtained substance of S2 and titanium dioxide accounting for 6 percent of the weight of the obtained substance, and carrying out high-speed shearing treatment on the blended substance by a high-speed shearing machine;
s4, carrying out double-screw extrusion treatment on the obtained substance in the step S3, then bracing, cooling and finally cutting to obtain the non-breathable biodegradable resin, wherein the temperature of the double-screw extrusion treatment is 120 ℃, the screw rotating speed is 350r/min, and the mold stripping pressure is 5 Mpa;
in the step S1, soaking PLA and PBAT in 75% ethanol for 5h, and then drying at 70 ℃ for 2 h;
when blending in the S3, adding titanium dioxide four times, wherein each time is 1min, the specific addition amount (mass concentration) of each time is 15%, 25%, 25% and 35%, and performing magnetic stirring at 50r/min in the whole adding process;
the high-speed shearing process in S3 includes the following two stages:
the first stage is as follows: treating at 300r/min for 30 min;
the second stage is 12000r/min for 10 min.
Example 2
The embodiment provides a preparation method of a non-breathable biodegradable resin, which comprises the following steps:
s1, mixing PLA and PBAT according to the proportion of 700g to 200g, drying at 65 ℃ for 2.5h, and spraying a sorbitol aqueous solution with the mass concentration of 50 percent accounting for 5 percent of the weight of the mixture on the surface of the mixture after drying;
s2, extruding the product obtained in the step S1 by a double screw at 160 ℃, the rotating speed of the screw is 370r/min, and the mold stripping pressure is 6.5 Mpa;
s3, blending the product obtained in the step S2 and titanium dioxide accounting for 7.5 percent of the weight of the product, and carrying out high-speed shearing treatment on the blend by using a high-speed shearing machine;
s4, carrying out double-screw extrusion treatment on the obtained substance in the step S3, then bracing, cooling and finally cutting to obtain the non-breathable biodegradable resin, wherein the temperature of the double-screw extrusion treatment is 130 ℃, the screw rotating speed is 320r/min, and the mold stripping pressure is 4 Mpa;
in the step S1, soaking PLA and PBAT in 85% ethanol for 4h, and then drying at 65 ℃ for 2.5 h;
when blending in the S3, adding titanium dioxide four times, wherein each time interval is 0.8min, the specific addition amount (mass concentration) of each time is 15%, 25%, 25% and 35%, and performing magnetic stirring at 80r/min in the whole adding process;
the high-speed shearing process in S3 includes the following two stages:
the first stage is as follows: treating at 400r/min for 25 min;
and in the second stage, 10000r/min treatment is carried out for 15 min.
Example 3
The embodiment provides a preparation method of a non-breathable biodegradable resin, which comprises the following steps:
s1, mixing PLA and PBAT according to a ratio of 900g to 300g, drying at 70 ℃ for 2h, and spraying a sorbitol aqueous solution with a mass concentration of 30% accounting for 3% of the weight of the blend on the surface of the blend after drying;
s2, extruding the product obtained in the step S1 by a double screw, wherein the temperature is 170 ℃, the rotating speed of the screw is 360r/min, and the mold stripping pressure is 5 Mpa;
s3, blending the obtained substance of S2 and titanium dioxide accounting for 9 percent of the weight of the obtained substance, and carrying out high-speed shearing treatment on the blended substance by a high-speed shearing machine;
s4, carrying out double-screw extrusion treatment on the obtained substance in the step S3, then bracing, cooling and finally cutting to obtain the non-breathable biodegradable resin, wherein the temperature of the double-screw extrusion treatment is 140 ℃, the screw rotating speed is 300r/min, and the mold stripping pressure is 3 Mpa;
in the step S1, soaking PLA and PBAT in 95% ethanol for 3h, and then drying at 60 ℃ for 3 h;
when blending in the S3, adding titanium dioxide four times, wherein the interval is 0.5min each time, the specific addition amount (mass concentration) of each time is 15%, 25%, 25% and 35%, and performing magnetic stirring at 100r/min in the whole adding process;
the high-speed shearing process in S3 includes the following two stages:
the first stage is as follows: treating at 500r/min for 20 min;
the second stage is 8000r/min for 20 min.
Example 4
The same as in example 1, except for the following differences:
the ratio of PLA and PBAT was 600 g:100 g.
Example 5
The same as in example 1, except for the following differences:
the mold release pressure in S2 was 9 MPa.
Example 6
The same as example 3, except for the following differences:
the ratio of PLA to PBAT was 900g: 350 g.
Example 7
The same as example 3, except for the following differences:
the mold release pressure in S2 was 4 MPa.
Example 8
The same as in example 1, except for the following differences:
5% of titanium dioxide is mixed in S3.
Example 9
The same as example 3, except for the following differences:
and 10% of titanium dioxide is mixed in the S3.
Example 10
The same as in example 1, except for the following differences:
titanium dioxide is not mixed in S3.
Example 11
The same as in example 1, except for the following differences:
and S2, stretching and cooling after twin-screw extrusion treatment, and finally cutting to obtain the non-breathable biodegradable resin.
Example 12
The same as in example 11 except for the following differences:
titanium dioxide in an amount of 6% of the product obtained in S1 was added during the twin-screw extrusion treatment in S2.
The performance of the non-breathable biodegradable resin obtained in the above examples was tested and the results are reported in the following table:
note: the resin is filmed by a film blowing machine, the film thickness is 0.03mm, and the performance of the resin is detected according to GB/T1040 and GB/T1043.
As can be seen from the table above, the non-breathable degradable resin prepared by the embodiments 1-3 has better tensile strength, impact strength and elongation at break;
example 1 is compared with example 4 to show that decreasing the PBAT ratio increases the values of the tensile strength, impact strength and elongation at break parameters, while example 3 is compared with example 6 to show that the PBAT ratio is not as high;
comparing the example 1 with the example 5, the result shows that the mold-stripping pressure in S2 is not too high easily, and comparing the example 3 with the example 7, the result shows that the mold-stripping pressure in S2 is not too low easily, and the quality parameter of the biodegradable resin can be optimized by maintaining the mold-stripping pressure at 5-8 MPa;
comparing the embodiment 1 with the embodiment 8 and the embodiment 9, the result shows that the optimal proportion of the titanium dioxide is 6-9%, and the titanium dioxide is not added in the embodiment 10, namely the content is 0, which shows that the addition of the titanium dioxide has a decisive effect on the improvement of the chromaticity of the resin, and the color can be ensured to be uniform in the optimal content range;
comparing example 1 with example 11, it is demonstrated that the second twin-screw extrusion treatment has a promoting effect on improving the quality characteristics of the resin, and at the same time, the addition of titanium dioxide also needs to be added in the second twin-screw extrusion treatment process to improve the chromaticity.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (10)
1. A preparation method of non-breathable biodegradable resin is characterized by comprising the following steps:
s1, mixing PLA and PBAT according to the mass ratio of 5-9: 1-3, drying, and spraying a sorbitol solution accounting for 3-7% of the weight of the blend on the surface of the mixture after drying;
s2, carrying out screw extrusion treatment on the product obtained in the step S1;
s3, blending the product obtained in the step S2 and titanium dioxide accounting for 6-9% of the weight of the product, and introducing the blend into a high-speed shearing machine for high-speed shearing treatment;
and S4, carrying out screw extrusion treatment on the substance obtained in the S3, then bracing, cooling and finally cutting to obtain the non-breathable biodegradable resin.
2. The method according to claim 1, wherein the solvent of the sorbitol solution is pure water with a mass concentration of 40-60%.
3. The method for preparing the non-breathable biodegradable resin as claimed in claim 1, wherein the PLA and the PBAT in S1 are soaked in 75-95% ethanol for 3-5 h and then dried, wherein the drying temperature is 60-70 ℃ and the drying time is 2-3 h.
4. The method for preparing the non-breathable biodegradable resin as claimed in claim 1, wherein the screw extrusion in S2 is twin-screw extrusion, the temperature is 150-170 ℃, the screw rotation speed is 360-380r/min, and the demolding pressure is 5-8 MPa.
5. The method for preparing a non-breathable biodegradable resin according to claim 1, wherein in the blending in S3, titanium dioxide is divided into four parts of 15%, 25%, 25% and 35% by mass, and the four parts are added to the product obtained in S2.
6. The method for preparing the non-breathable biodegradable resin according to claim 5, wherein the time interval for adding the titanium dioxide in portions is 0.5-1 min, and the stirring is continued for 50-100 r/min during the adding process.
7. The method of claim 6, wherein the stirring during the addition of titanium dioxide is magnetic stirring.
8. The method of claim 1, wherein the high shear treatment in S3 is performed in two stages:
the first stage is as follows: treating for 20-30 min at 300-500 r/min;
the second stage is 8000-12000 r/min for 10-15 min.
9. The method for preparing the non-breathable biodegradable resin as claimed in claim 1, wherein the screw extrusion in S4 is twin-screw extrusion, the temperature is 120-140 ℃, the screw rotation speed is 300-350r/min, and the demolding pressure is 3-5 MPa.
10. A non-breathable biodegradable resin, characterized by being produced by the production method according to claim 1.
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| CN109111710A (en) * | 2018-08-07 | 2019-01-01 | 万卓（武汉）新材料有限公司 | A kind of heat resistant type PLA base degradation plastic bottle and preparation method thereof |
| CN109401227A (en) * | 2018-10-25 | 2019-03-01 | 南京五瑞生物降解新材料研究院有限公司 | Using the PLA/PBAT blending and modifying Biodegradable resin and preparation method thereof of chain extender preparation |
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Application publication date: 20210504 |