Polylactic acid composition and method for preparing same
The polylactic acid composition, formed by reacting specific compounds and optionally including rare earth oxides, addresses the issues of flame retardancy and toughness in polymeric materials, enhancing both properties effectively.
Patent Information
- Application Number
- JP2024009659
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- Priority Date
- 2023-10-17
- Filing Date
- 2024-01-25
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2044-01-25
AI Technical Summary
Existing polymeric materials lack adequate flame retardancy and toughness, and current flame retardants either require high additive amounts or have poor compatibility with polymers, affecting mechanical properties.
A polylactic acid composition is developed by reacting a compound represented by formula (A) with a compound represented by formula (B), optionally with rare earth oxides and auxiliary agents, in specific molar ratios and conditions, to enhance flame retardancy and toughness.
The composition achieves both good flame retardancy and high toughness, improving mechanical properties while maintaining compatibility with polymeric materials.
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Abstract
Description
[Technical Field]
[0001] The present invention relates to a polylactic acid composition and a method for preparing the same. [Background technology]
[0002] Polymeric materials are widely used in fields such as automobiles, construction, home appliances, and agriculture. However, most polymeric materials have poor flame retardancy and require the addition of flame retardants for practical use. Combining single-component flame retardants results in a high additive amount, resulting in a reduced flame retardant effect. Multi-component composite flame retardants have poor compatibility with polymeric materials, affecting the mechanical properties of the polymeric materials.
[0003] CN114805816A discloses a method for preparing a flame retardant, which comprises dissolving polymethylhydrosiloxane in a solvent, adding linear alkenyloxypentachlorocyclotriphosphazene and a catalyst, reacting the mixture with stirring for 10 to 40 hours, removing the solvent, and then drying to obtain a polymeric flame retardant.
[0004] CN111875648A discloses a method for preparing a bio-based polymeric flame retardant, which comprises adding 10-30 g of tannic acid and 5-20 mL of triethylamine to 50-200 mL of acetonitrile to obtain a mixture, heating the mixture to 30-45°C, adding 10-40 mL of hexachlorocyclotriphosphazene to the mixture, and heating the mixture at 50°C for 1-3 hours to obtain a mixed solution containing tannic acid chlorophosphazene ester, adding 10-30 g of m-phenylenediamine to the mixed solution, heating to 60-80°C, reacting for 2-4 hours, filtering, rinsing with acetonitrile to remove triethylamine salt and unreacted raw materials, and drying to obtain a bio-based polymeric flame retardant.
[0005] There is room for further improvement in the flame retardancy and toughness of the flame retardants. Summary of the Invention
[0006] In view of this, one object of the present invention is to provide a polylactic acid composition having both good flame retardancy and toughness, and another object of the present invention is to provide a method for preparing the polylactic acid composition.
[0007] The above object can be achieved by the following configuration.
[0008] In one aspect, the present invention provides a polylactic acid composition comprising a polymeric material and a reaction product obtained by reacting a compound represented by formula (A) with a compound represented by formula (B), wherein the polymeric material contains polylactic acid. TIFF0007729931000001.tif86170 (where R a ~R f are each independently selected from H, C1-C10 alkyl, and halogen; Here, X1 to X3 are each independently selected from H and C1 to C3 alkyl, and n is selected from an integer of 0 to 10. In the polylactic acid composition according to the present invention, the molar ratio of the compound represented by formula (A) to the compound represented by formula (B) is preferably 6:(25-80).
[0009] In the polylactic acid composition according to the present invention, n is preferably selected from integers of 0 to 7, and X1 to X3 are each independently selected from H.
[0010] According to the polylactic acid composition of the present invention, the reaction product is preferably contained in an amount of 1 to 30 parts by weight based on 100 parts by weight of the polymer material.
[0011] In the polylactic acid composition according to the present invention, the content of the polylactic acid in the polymer material is preferably 40 wt % or more.
[0012] According to the polylactic acid composition of the present invention, the polymer material preferably further contains one or more of polyethylene, polypropylene, polyvinyl chloride, polyester-based materials, and epoxy resins.
[0013] According to the polylactic acid composition of the present invention, preferably, the polylactic acid composition further contains a rare earth oxide, and the rare earth oxide is contained in an amount of 0.3 to 2 parts by weight based on 100 parts by weight of the polymer material.
[0014] The rare earth oxide is one or more selected from lanthanum oxide, cerium oxide, and yttrium oxide.
[0015] In another aspect, the present invention provides a method for producing a pharmaceutical composition comprising: A step of melting raw materials containing a polymer material and a reaction product to obtain a polylactic acid composition. and a method for preparing the polylactic acid composition, comprising:
[0016] According to the preparation method of the present invention, preferably A step of reacting a compound represented by formula (A) with a compound represented by formula (B) in the presence of a solvent and an acid binder to obtain a reaction product, the solvent is one or more selected from chloromethane, methylene chloride, chloroform, tetrachloroform, ethyl chloride, dichloroethane, trichloroethane, tetrachloroethane, chloropropane, dichloropropane, trichloropropane, tetrachloropropane, ethyl acetate, dimethyl sulfoxide, and acetone; the acid binder is one or more selected from the group consisting of a tertiary amine compound, pyridine, and tetraethylenepentamine; the molar ratio of the compound represented by formula (A) to the acid binder is 6:(30 to 90); a step in which the reaction temperature is -10 to 10°C and the reaction time is 24 to 80 hours; Further includes:
[0017] According to the preparation method of the present invention, the melting temperature is preferably 165 to 195°C, the melting is carried out with stirring, and the screw rotation speed is preferably 30 to 120 rpm.
[0018] The polylactic acid composition according to the present invention has both good flame retardancy and relatively high toughness. DETAILED DESCRIPTION OF THE INVENTION
[0019] The present invention will be further described below in conjunction with specific examples, but the scope of protection of the present invention is not limited thereto.
[0020] <Polylactic acid composition> The polylactic acid composition according to the present invention comprises a reaction product obtained by reacting a polymeric material with a compound represented by formula (A) and a compound represented by formula (B). In some embodiments, the polylactic acid composition may further comprise one or more of a rare earth oxide and an auxiliary agent.
[0021] The polymeric material according to the present invention comprises polylactic acid. The content of polylactic acid in the polymeric material is 40 wt% or more, preferably 50 wt% or more, more preferably 70 wt% or more. The content of polylactic acid in the polymeric material is less than 80 wt%, preferably less than 90 wt%, more preferably less than 100 wt%. In some embodiments, the polymeric material is polylactic acid. In other embodiments, the polymeric material further comprises one or more of polyethylene, polypropylene, polyvinyl chloride, a polyester-based material, and an epoxy resin. The polyester-based material may be an aromatic polyester or a linear polyester. In some embodiments, the polyester-based material is polycarbonate. In other embodiments, the polyester-based material is obtained by copolymerizing an aromatic dibasic acid, a linear dibasic acid, and a linear diol. In some other embodiments, the polyester-based material is obtained by copolymerizing a linear dibasic acid, an aromatic diol, or a linear diol. Examples of polyester-based materials include, but are not limited to, polybutylene adipate / terephthalate copolymer and polybutylene succinate.
[0022] Formula (A) is specifically shown below.
[0023] TIFF0007729931000002.tif46170In formula (A), R a ~R f are each independently selected from H, C1 to C10 alkyl, and halogen. a ~R f are each independently selected from H, C1 to C6 alkyl, and halogen. More preferably, R a ~R f are each independently selected from H, C1-C3 alkyl, and halogen.
[0024] In the present invention, the C1-C10 alkyl may be a chain alkyl or a cycloalkyl. In some embodiments, it is a chain alkyl. The chain alkyl may be a linear chain alkyl or a branched chain alkyl. In some embodiments, the C1-C10 alkyl is a linear chain alkyl. Specific examples of C1-C10 alkyl include, but are not limited to, methyl, ethyl, propyl, isopropyl, butyl, methylpropyl, pentyl, methylbutyl, dimethylpropyl, ethylpropyl, hexyl, methylpentyl, dimethylbutyl, ethylbutyl, cyclopropyl, and cyclopentyl.
[0025] Illustrative examples of halogens include, but are not limited to, fluorine, chlorine, bromine, and iodine. Preferably, the halogen is chlorine.
[0026] In some embodiments, R a ~R f At least three of R are halogen. a ~R f At least four of R are halogen. a ~R f At least five of these are halogens.
[0027] In some embodiments, R a and R b At least one of R is halogen;c and R d At least one of R is halogen; e and R f At least one of is a halogen.
[0028] In some embodiments, R a ~R f are all halogens.
[0029] Illustrative examples of compounds represented by formula (A) include, but are not limited to, hexachlorocyclotriphosphazene.
[0030] Formula (B) is specifically shown below.
[0031] TIFF0007729931000003.tif36170X1 to X3 are each independently selected from H and C1 to C3 alkyl, and n is an integer selected from 0 to 10.
[0032] X1-X3 are each independently selected from H and C1-C3 alkyl. In some embodiments, X1-X3 are each independently selected from H. The C1-C3 alkyl may be a chain alkyl or a cycloalkyl. In some embodiments, the C1-C3 alkyl is a chain alkyl. The chain alkyl may be a linear chain alkyl or a branched chain alkyl. In some embodiments, the C1-C3 alkyl is a linear chain alkyl. Examples of C1-C3 alkyl include, but are not limited to, methyl, ethyl, propyl, isopropyl, and cyclopropyl.
[0033] n is selected from an integer from 0 to 10. In some embodiments, n is 0. In other embodiments, n is selected from an integer from 1 to 7. In other embodiments, n is selected from an integer from 2 to 5.
[0034] Illustrative examples of compounds represented by formula (B) include, but are not limited to, ethylenediamine, propylenediamine, butanediamine, pentylenediamine, and hexamethylenediamine.
[0035] The molar ratio of the compound represented by formula (A) to the compound represented by formula (B) may be 6:(25 to 80), preferably 6:(30 to 70), and more preferably 6:(40 to 60).
[0036] The amount of the reaction product obtained by reacting the compound represented by formula (A) with the compound represented by formula (B) is 1 to 30 parts by weight, preferably 5 to 25 parts by weight, and more preferably 10 to 20 parts by weight, based on 100 parts by weight of the polymer material.
[0037] The rare earth oxide according to the present invention is one or more selected from lanthanum oxide, cerium oxide, and yttrium oxide. The mass ratio of the reaction product obtained by reacting the compound represented by formula (A) with the compound represented by formula (B) to the rare earth oxide may be (3-20):1, preferably (5-15):1, and more preferably (8-12):1.
[0038] The amount of rare earth oxide is 0.3 to 2 parts by weight, preferably 0.5 to 1.5 parts by weight, and more preferably 0.8 to 1.2 parts by weight, based on 100 parts by weight of the polymer material.
[0039] The auxiliary agent according to the present invention may be one or more selected from soybean oil, epoxidized soybean oil, tributyl citrate, acetyl tributyl citrate, antioxidants and plasticizers.
[0040] The amount of the auxiliary agent may be 0.1 to 2 parts by weight, preferably 0.5 to 1.5 parts by weight, and more preferably 0.5 to 1 part by weight, based on 100 parts by weight of the polymer material.
[0041] <Method for preparing polylactic acid composition> The method for preparing a polylactic acid composition according to the present invention includes melting raw materials containing a polymeric material and a reaction product to obtain a polylactic acid composition. The raw materials may further contain a rare earth oxide and an auxiliary agent. In some embodiments, the method further includes granulating the melted product obtained by melting.
[0042] The reaction product is a reaction product obtained by reacting a compound represented by formula (A) with a compound represented by formula (B). The chemical structures of the compound represented by formula (A) and the compound represented by formula (B) and the details of their amounts used are as described above and will not be repeated here. The details of the selection and amount of each raw material are as described above and will not be repeated here.
[0043] The melting temperature may be 165 to 195° C., and preferably 170 to 180° C. The melting time may be 5 to 15 minutes, and preferably 7 to 10 minutes.
[0044] The melting is carried out with stirring, for example, by using a screw extruder, and the screw rotation speed may be 30 to 120 rpm, and preferably 50 to 100 rpm.
[0045] In some embodiments, the method further comprises reacting a compound of Formula (A) with a compound of Formula (B).
[0046] The compound of Formula (A) and the compound of Formula (B) may be reacted in the presence of a solvent. The solvent may be one or more selected from chloromethane, methylene chloride, chloroform, tetrachloroform, ethyl chloride, dichloroethane, trichloroethane, tetrachloroethane, chloropropane, dichloropropane, trichloropropane, tetrachloropropane, ethyl acetate, dimethyl sulfoxide, and acetone. In some embodiments, the solvent is methylene chloride.
[0047] The compound represented by formula (A) and the compound represented by formula (B) may be reacted in the presence of an acid binder. The acid binder may be one or more selected from a tertiary amine compound, pyridine, and tetraethylenepentamine. The tertiary amine compound may be one or more selected from triethylamine and N,N-diisopropylethylamine.
[0048] The compound of formula (A) and the compound of formula (B) may be reacted under the protection of an inert gas, examples of which include, but are not limited to, nitrogen gas, helium gas, neon gas, and argon gas.
[0049] The reaction temperature may be -10 to 10°C, preferably -5 to 5°C, and more preferably -2 to 2°C.
[0050] The reaction time may be 24 to 80 hours, preferably 30 to 60 hours, and more preferably 40 to 50 hours.
[0051] The molar ratio of the compound represented by formula (A) to the acid binder is 6:(30 to 90), preferably 6:(40 to 80), and more preferably 6:(50 to 70).
[0052] The amount of the solvent used is 100 to 600 mL, preferably 200 to 500 mL, and more preferably 300 to 400 mL, based on 0.06 mol of the compound represented by the formula (A).
[0053] Specifically, a second reactant containing a compound of formula (A) and a portion of the solvent is added dropwise to a first reactant containing a compound of formula (B), an acid binder, and the remaining solvent. This step may be carried out under the protection of an inert gas. Examples of inert gases include, but are not limited to, nitrogen gas, helium gas, neon gas, and argon gas.
[0054] The ratio of the solvent in the second reactant to the total volume of the solvent is 0.05 to 0.6:1, and preferably 0.2 to 0.4:1.
[0055] In some embodiments, the method further comprises centrifuging the resulting material and filtering it to obtain a filter cake. The filter cake is then vacuum-dried at 30 to 70°C, preferably 40 to 60°C, for 7 to 15 hours, preferably 9 to 12 hours, to obtain the reaction product. "Vacuum" refers to a relative vacuum of -0.05 to -0.1 MPa.
[0056] The raw materials used in the following examples and comparative examples are introduced below.
[0057] Hexachlorocyclotriphosphazene was purchased from Shanghai Macklin Biochemical Technology Co., Ltd.
[0058] The polylactic acid was purchased from Total, model number L175.
[0059] Polybutylene adipate / terephthalate copolymer was purchased from Xinjiang Blue Ridge Tunhe Energy Co., Ltd., model number TH801T.
[0060] The measurement methods used in the following examples and comparative examples are described below.
[0061] Oxygen index performance measurement: Measured using an oxygen index meter in accordance with the method specified in GB / T2406.1-2008.
[0062] Vertical combustion performance measurement: Measured using a horizontal and vertical combustion tester in accordance with the method specified in GB / T2408-2021.
[0063] Breaking elongation: measured using a universal testing machine in accordance with the method specified in GB / T1040.1-2018, where the tensile speed is 2.0 mm / min.
[0064] Example 1 A first mixture was obtained by mixing 0.5 mol of butanediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. A first reactant was obtained by mixing the first mixture and the second mixture. A second reactant was obtained by dissolving 0.06 mol of hexachlorocyclotriphosphazene in 100 mL of methylene chloride.
[0065] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0066] 100 parts by weight of polylactic acid, 10 parts by weight of the reaction product, 1 part by weight of cerium oxide, and 0.5 parts by weight of epoxidized soybean oil were melted for 7 minutes at a temperature of 175°C and a screw rotation speed of 80 rpm to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0067] The performance of the polylactic acid composition is shown in Table 1.
[0068] Example 2 A first mixture was obtained by mixing 0.5 mol of ethylenediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. The first mixture and the second mixture were mixed to obtain a first reactant. 0.06 mol of hexachlorocyclotriphosphazene was dissolved in 100 mL of methylene chloride to obtain a second reactant.
[0069] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0070] 100 parts by weight of polylactic acid, 10 parts by weight of the reaction product, 1 part by weight of cerium oxide, and 0.5 parts by weight of epoxidized soybean oil were melted for 7 minutes at a temperature of 175°C and a screw rotation speed of 80 rpm to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0071] The performance of the polylactic acid composition is shown in Table 1.
[0072] Example 3 A first mixture was obtained by mixing 0.5 mol of propylenediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. A first reactant was obtained by mixing the first mixture and the second mixture. A second reactant was obtained by dissolving 0.06 mol of hexachlorocyclotriphosphazene in 100 mL of methylene chloride.
[0073] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0074] 100 parts by weight of polylactic acid, 10 parts by weight of the reaction product, 1 part by weight of cerium oxide, and 0.5 parts by weight of epoxidized soybean oil were melted for 7 minutes at a temperature of 175°C and a screw rotation speed of 80 rpm to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0075] The performance of the polylactic acid composition is shown in Table 1.
[0076] Example 4 A first mixture was obtained by mixing 0.5 mol of butanediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. A first reactant was obtained by mixing the first mixture and the second mixture. A second reactant was obtained by dissolving 0.06 mol of hexachlorocyclotriphosphazene in 100 mL of methylene chloride.
[0077] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0078] 100 parts by weight of polylactic acid, 11 parts by weight of the reaction product, and 0.5 parts by weight of epoxidized soybean oil were melted for 7 minutes at a temperature of 175°C and a screw rotation speed of 80 rpm to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0079] The performance of the modified polylactic acid material is shown in Table 1.
[0080] Comparative Example 1 100 parts by weight of polylactic acid was melted for 7 minutes at a temperature of 175°C and a screw rotation speed of 80 rpm to obtain a molten product, which was then granulated to obtain a polylactic acid material.
[0081] The performance of the polylactic acid material is shown in Table 1.
[0082] TIFF0007729931000004.tif47170 Example 5 A first mixture was obtained by mixing 0.5 mol of butanediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. A first reactant was obtained by mixing the first mixture and the second mixture. A second reactant was obtained by dissolving 0.06 mol of hexachlorocyclotriphosphazene in 100 mL of methylene chloride.
[0083] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0084] 70 parts by weight of polylactic acid, 30 parts by weight of polybutylene adipate / terephthalate copolymer ester, 10 parts by weight of the reaction product, 1 part by weight of cerium oxide, and 0.5 parts by weight of epoxidized soybean oil were melted at a temperature of 175°C and a screw rotation speed of 80 rpm for 7 minutes to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0085] The performance of the polylactic acid composition is shown in Table 2.
[0086] Example 6 A first mixture was obtained by mixing 0.5 mol of ethylenediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. The first mixture and the second mixture were mixed to obtain a first reactant. 0.06 mol of hexachlorocyclotriphosphazene was dissolved in 100 mL of methylene chloride to obtain a second reactant.
[0087] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0088] 70 parts by weight of polylactic acid, 30 parts by weight of polybutylene adipate / terephthalate copolymer ester, 10 parts by weight of the reaction product, 1 part by weight of cerium oxide, and 0.5 parts by weight of epoxidized soybean oil were melted at a temperature of 175°C and a screw rotation speed of 80 rpm for 7 minutes to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0089] The performance of the polylactic acid composition is shown in Table 2.
[0090] Example 7 A first mixture was obtained by mixing 0.5 mol of propylenediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. A first reactant was obtained by mixing the first mixture and the second mixture. A second reactant was obtained by dissolving 0.06 mol of hexachlorocyclotriphosphazene in 100 mL of methylene chloride.
[0091] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0092] 70 parts by weight of polylactic acid, 30 parts by weight of polybutylene adipate / terephthalate copolymer ester, 10 parts by weight of the reaction product, 1 part by weight of cerium oxide, and 0.5 parts by weight of epoxidized soybean oil were melted at 175°C and a screw rotation speed of 80 rpm for 7 minutes to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0093] The performance of the polylactic acid composition is shown in Table 2.
[0094] Example 8 A first mixture was obtained by mixing 0.5 mol of butanediamine and 100 mL of methylene chloride. A second mixture was obtained by mixing 0.6 mol of triethylamine and 100 mL of methylene chloride. A first reactant was obtained by mixing the first mixture and the second mixture. A second reactant was obtained by dissolving 0.06 mol of hexachlorocyclotriphosphazene in 100 mL of methylene chloride.
[0095] The second reactant was added dropwise to the first reactant under a nitrogen gas atmosphere, and the mixture was allowed to react at 0°C for 48 hours. The mixture was then centrifuged and filtered to obtain a filter cake, which was then vacuum-dried at 50°C for 10 hours to obtain the reaction product.
[0096] 70 parts by weight of polylactic acid, 30 parts by weight of polybutylene adipate / terephthalate copolymer ester, 11 parts by weight of the reaction product, and 0.5 parts by weight of epoxidized soybean oil were melted at 175°C and a screw rotation speed of 80 rpm for 7 minutes to obtain a molten product. The molten product was granulated to obtain a polylactic acid composition.
[0097] The performance of the polylactic acid composition is shown in Table 2.
[0098] Comparative Example 2 70 parts by weight of polylactic acid and 30 parts by weight of polybutylene adipate / terephthalate copolymer were melted at 175°C and a screw rotation speed of 80 rpm for 7 minutes to obtain a molten product. The molten product was then granulated to obtain a composite polylactic acid material.
[0099] The performance of the composite polylactic acid material is shown in Table 2.
[0100] TIFF0007729931000005.tif47170The present invention is not limited to the above-described embodiments, and all modifications, improvements, substitutions, etc. that may occur to those skilled in the art are included within the scope of the present invention, as long as they do not deviate from the spirit of the present invention.
Claims
1. A polylactic acid composition comprising a polymer material and a reaction product obtained by reacting a compound represented by formula (A) with a compound represented by formula (B), The polylactic acid composition further contains a rare earth oxide, and the rare earth oxide is contained in an amount of 0.3 to 2 parts by weight based on 100 parts by weight of the polymer material; the rare earth oxide is one or more selected from lanthanum oxide, cerium oxide, and yttrium oxide; A polylactic acid composition, wherein the polymer material contains polylactic acid. (where R a ~R f are each independently selected from H, C1-C10 alkyl, and halogen; Here, X 1 ~X 3 are each independently selected from H and C1-C3 alkyl, and n is selected from an integer of 0 to 10.
2. 2. The polylactic acid composition according to claim 1, wherein the molar ratio of the compound represented by formula (A) to the compound represented by formula (B) is 6:(25-80).
3. n is selected from integers of 0 to 7, and X 1 ~X 3 The polylactic acid composition according to claim 1, wherein each of the groups is independently selected from H.
4. 2. The polylactic acid composition according to claim 1, wherein the reaction product is contained in an amount of 1 to 30 parts by weight based on 100 parts by weight of the polymer material.
5. 2. The polylactic acid composition according to claim 1, wherein the content of said polylactic acid in the polymer material is 40 wt % or more.
6. The polylactic acid composition according to claim 1, wherein the polymer material further comprises one or more of polyethylene, polypropylene, polyvinyl chloride, polyester-based materials, and epoxy resins.
7. 2. The method for preparing a polylactic acid composition according to claim 1, comprising the step of melting raw materials containing a polymer material and a reaction product to obtain a polylactic acid composition.
8. A step of reacting a compound represented by (A) with a compound represented by (B) in the presence of a solvent and an acid binder to obtain a reaction product, the solvent is one or more selected from chloromethane, methylene chloride, chloroform, tetrachloroform, ethyl chloride, dichloroethane, trichloroethane, tetrachloroethane, chloropropane, dichloropropane, trichloropropane, tetrachloropropane, ethyl acetate, dimethyl sulfoxide, and acetone; the acid binder is one or more selected from the group consisting of a tertiary amine compound, pyridine, and tetraethylenepentamine; the molar ratio of the compound represented by formula (A) to the acid binder is 6:(30-90); a step in which the reaction temperature is −10 to 10° C. and the reaction time is 24 to 80 hours; 8. The method of claim 7, comprising:
9. 8. The method according to claim 7, wherein the melting temperature is 165-195°C, the melting is carried out with stirring, and the screw speed is 30-120 rpm.
Citation Information
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