Organic nucleating agent for preparing heat resistant polylactic acid resin and preparation method thereof

A technology of polylactic acid resin and organic nucleating agent, applied in the field of polylactic acid resin preparation, can solve the problems of restricting the processing and application of polylactic acid resin products, unable to realize industrialized production, insufficient heat resistance of molded products, etc., so as to improve nucleation Efficiency, shortened production cycle, and improved mechanical properties

Inactive Publication Date: 2020-03-27
BENGBU COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Polylactic acid resin is a bio-based and degradable polymer material with excellent physical and mechanical properties, biodegradability and biocompatibility. It has great potential in the fields of agriculture, packaging materials, daily life, clothing and biomedical materials. It has a good application prospect, but its application is still subject to many constraints, the most important of which is the poor heat resistance of polylactic acid resin. The application of resin has been greatly restricted
[0003] In the prior art, in order to improve the heat resistance of biopolymer materials, it is common practice to add nucleating agents during the preparation process; 3 、TiO 2 and BaSO 4 Inorganic salt is added in the polylactic acid resin as nucleating agent, but can't realize suitability for industrialized production so far; Also someone adopts talcum powder as nucleating agent, for example, the patent that publication number is CN103467947A discloses a kind of using talcum powder as filler and nucleating agent. The polylactic acid resin of agent and preparation method thereof, but the polylactic acid resin of making like this is owing to adding a large amount of talcum powder, and its product toughness is relatively poor, and the heat resistance of product is still unsatisfactory
[0004] Therefore, polylactic acid resin has slow crystallization rate, long molding cycle, and insufficient heat resistance of molded products during use, which seriously restricts the processing and application of polylactic acid resin products. This urgent technical problem has become a hot issue in the field of polylactic acid resin preparation.

Method used

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  • Organic nucleating agent for preparing heat resistant polylactic acid resin and preparation method thereof
  • Organic nucleating agent for preparing heat resistant polylactic acid resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The organic nucleating agent for preparing heat-resistant polylactic acid resin is prepared by the following method:

[0027] Step 1) Put 100 mL of thionyl chloride into the reaction vessel, divide 20 g of sodium terephthalate powder into several parts, and add 1 to 2 g in each part gradually to obtain a mixed solution; 0.2% butyl ammonium titanate or dibutyltin dilaurate or stannous chloride as a catalyst of phthalic acid metal salt, react to obtain terephthaloyl chloride;

[0028] Step 2) a certain proportion of alkylcyclohexylamine, ethyl acetate and DMF are mixed, and the mol ratio of alkylcyclohexylamine, ethyl acetate and DMF described in this embodiment is 4:1:1, and then the Terephthaloyl chloride is slowly added dropwise therein, and the said terephthaloyl chloride is controlled to be added dropwise within 0.5h, and component A is obtained after the reaction;

[0029] Step 3) Take polyethylene glycol with a weight fraction of 65% and heat it to 30° C., slowly ...

Embodiment 2

[0033] The organic nucleating agent for preparing heat-resistant polylactic acid resin is prepared by the following method:

[0034] Step 1) Put 110mL of phosphorus pentachloride into the reaction vessel, divide 28g of magnesium terephthalate powder into several parts, and add 1-2g of each part gradually to obtain a mixed solution; when heated to 120°C, add a mass fraction of Terephthalic acid metal salt 3% butyl ammonium titanate, dibutyltin dilaurate or stannous chloride are used as catalysts to react to obtain terephthaloyl chloride;

[0035] Step 2) a certain proportion of alkylcyclohexylamine, ethyl acetate and DMF are mixed, the mol ratio of alkylcyclohexylamine, ethyl acetate and DMF described in the present embodiment is 5:2:1, then described Terephthaloyl chloride is slowly added dropwise therein, and the described terephthaloyl chloride is controlled to be added dropwise within 1.5h, and component A is obtained after the reaction;

[0036] Step 3) Take polyethylene ...

Embodiment 3

[0039] The organic nucleating agent for preparing heat-resistant polylactic acid resin is prepared by the following method:

[0040] Step 1) Put 90mL of phosphorus trichloride into the reaction vessel, divide 15g of sodium terephthalate powder into multiple portions, and add 1-2g of each portion gradually to obtain a mixed solution; when heated to 110°C, add the mass fraction of 1% butyl ammonium titanate, dibutyltin dilaurate or tin protochloride as a catalyst to obtain terephthaloyl chloride;

[0041] Step 2) a certain proportion of alkylcyclohexylamine, ethyl acetate and DMF are mixed, and the mol ratio of alkylcyclohexylamine, ethyl acetate and DMF described in this embodiment is 4:2.5:1, and then described Terephthaloyl chloride is slowly added dropwise therein, and the described terephthaloyl chloride is controlled to be added dropwise within 1 hour, and component A is obtained after the reaction;

[0042] Step 3) Take polyethylene glycol with a weight fraction of 85% a...

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Abstract

The invention discloses an organic nucleating agent for preparing heat resistant polylactic acid resin and a preparation method thereof. The preparation method comprises following steps: (1) mixing terephthalate of metals and a chlorination agent to obtain a mixed solution, adding a catalyst, carrying out reactions to obtain terephthaloyl chloride; (2) mixing alkyl cyclohexane, ethyl acetate, andDMF according to a certain ratio, dropwise adding terephthaloyl chloride into the mixture, and carrying out reactions to obtain a component A; (3) heating polyethylene glycol with a weight percentageof 65-85% to a temperature of 30 to 75 DEG C, and slowly adding the component A into polyethylene glycol under stirring; and (4) adding disodium salicylate into the solution obtained in the step (3),and then mixing the solution with resin emulsion to obtain the nucleating agent. Terephthalate of metals and the chlorination agent are mixed to obtain the mixed solution, then disodium salicylate isadded, the heatproof property and moulding property of polylactic acid resin are improved, and the processing and production period is shortened.

Description

technical field [0001] The invention relates to the field of polylactic acid resin preparation, in particular to an organic nucleating agent for preparing heat-resistant polylactic acid resin and a preparation method thereof. Background technique [0002] Polylactic acid resin is a bio-based and degradable polymer material with excellent physical and mechanical properties, biodegradability and biocompatibility. It has great potential in the fields of agriculture, packaging materials, daily life, clothing and biomedical materials. It has a good application prospect, but its application is still subject to many constraints, the most important of which is the poor heat resistance of polylactic acid resin. The application of resin has been greatly restricted. [0003] In the prior art, in order to improve the heat resistance of biopolymer materials, it is common practice to add nucleating agents during the preparation process; 3 、TiO 2 and BaSO 4 Inorganic salt is added in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08L63/00C08L75/04C08L71/02C08K5/098C08K5/20
CPCC08K5/098C08K5/20C08L63/00C08L67/04C08L71/02C08L75/04C08L2201/08C08L2205/24
Inventor 吴景梅朱俊杰韩言松刘保杰
Owner BENGBU COLLEGE
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