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Ureas nucleating agent-containing polylactic acid composite and preparation method thereof

A polylactic acid and nucleating agent technology, applied in the field of polylactic acid nucleating agents, can solve problems such as insufficient nucleation effect, unenvironmental protection in the application process, instability of polylactic acid, etc., to achieve significant nucleation effect, low cost, and responsive simple and fast effect

Inactive Publication Date: 2012-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] It can be seen that the existing nucleating agents still have various deficiencies such as insufficiently significant nucleating effect or large dosage, complicated preparation, high cost, self-instability or instability of polylactic acid, and unenvironmental protection in the application process, which cannot meet the needs of the polylactic acid industry. needs

Method used

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  • Ureas nucleating agent-containing polylactic acid composite and preparation method thereof
  • Ureas nucleating agent-containing polylactic acid composite and preparation method thereof
  • Ureas nucleating agent-containing polylactic acid composite and preparation method thereof

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preparation example Construction

[0046] The steps of the preparation method of the polylactic acid composition containing urea nucleating agent are as follows:

[0047] 1) React amine and isocyanate in solvent A at 10-40°C for 0.5-3 hours, the molar ratio of isocyanate to amine is 0.4-1.5; after the reaction, filter the reaction product, and use solvent B and solvent C in sequence Wash and dry the filter residue under vacuum at 60-80°C for 8-48 hours to obtain a powdered urea nucleating agent; wherein, solvent A is N,N-dimethylacetamide or N,N-dimethylformamide , the solvent consumption is 3.5-6 times of the volume of isocyanate; Solvent B is chloroform, n-hexane, carbon tetrachloride, benzene or toluene, and the solvent consumption is 5-10 times of solvent A; Solvent C is water, methanol, ethanol, propylene glycol Alcohol or isopropanol, the amount of solvent is 5-10 times that of solvent A;

[0048] 2) Add polylactic acid and 0.1-5% urea nucleating agent of the mass of polylactic acid, or polylactic acid, ...

Embodiment 1

[0062] Embodiment 1: Preparation of nucleating agent NA1

[0063] Preparation process: 3.606g (60.0mmol) of ethylenediamine was dissolved in 15mL of N,N-dimethylacetamide, and 7.147g (60.0mmol, 6.54ml) of phenylisocyanate was dissolved in 15mL of N , N-dimethylacetamide dubbed solution. During the dropping process, the temperature was kept below 40°C, and after the dropping was completed, the reaction was continued for 30 minutes. After the reaction, the reactant was filtered with a Buchner funnel, and washed with 150ml (five times the volume of N,N-dimethylacetamide) chloroform and 150ml of ethanol successively, and the filter residue was vacuum-dried at 60-80°C for 8 -48 hours to constant weight, to obtain a white powder, that is, the nucleating agent NA1, with a yield of 93.1%.

[0064] The structural formula of the nucleating agent NA1 is

[0065]

[0066] The H NMR spectrum of the nucleating agent NA1 is shown in Figure 1(a).

Embodiment 2

[0067] Embodiment 2: prepare nucleating agent NA2

[0068] Preparation process: Dissolve 4.408g (50.0mmol) of butanediamine in 15mL of N,N-dimethylacetamide, and add dropwise 8.934g (75.0mmol, 8.17ml) of phenylisocyanate dissolved in 15mL of N , N-dimethylacetamide dubbed solution. During the dropwise addition, keep the temperature below 30° C., and continue the reaction for 2 hours after the dropwise addition. After the reaction, the reactant was filtered with a Buchner funnel, washed with 150ml of chloroform and 150ml of ethanol in turn, and the filter residue was vacuum-baked at 60-80°C for 8-48 hours to constant weight to obtain a white powder, that is, the nucleating agent NA2 , yield 95.4%.

[0069] The structural formula of the nucleating agent NA2 is

[0070]

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Abstract

The invention discloses ureas nucleating agent-containing polylactic acid composite and a preparation method of the ureas nucleating agent-containing polylactic acid composite. The ureas nucleating agent-containing polylactic acid composite consists of polylactic acid, ureas nucleating agent or polylactic acid, ureas nucleating agent and plasticizer, wherein the weight of the nucleating agent is 0.1-5% of that of the polylactic acid, the plasticizer is tributyl citrate, acetyl tributyl citrate, polyethylene glycol or the mixture of the tributyl citrate, the acetyl tributyl citrate and the polyethylene glycol, and the weight of the plasticizer is 5-20% of that of the polylactic acid. The nucleating agent contains one or two urea bond(s), and is obtained by reacting unitary or binary secondary amine or primary amine, ramification of the unitary or binary secondary amine or the primary amine with mono-isocyanate or diisocyanate. The nucleating agent has the characteristics of being simple in preparation, easy for industrialization, high-efficiency, and low in price, is used for the polylactic resin, the crystallization of the polylactic acid can be intensively promoted due to the heterogeneous nucleation effect, the crystalline grain of the polylactic acid can be refined, and the heat resistance and the mechanical property of the polylactic acid can be improved. The nucleating agent is coupled with the plasticizer, so that the plasticity and the toughness of the polylactic acid can be further improved, and the application range of the composite can be widened.

Description

technical field [0001] The invention relates to the technical field of polylactic acid nucleating agents, in particular to a polylactic acid composition containing a nucleating agent. Background technique [0002] Polylactic acid is a bio-based biodegradable material with broad application prospects. However, polylactic acid has disadvantages such as high brittleness and poor heat resistance. The heat distortion temperature of polylactic acid products obtained by injection molding is only about 58°C, which is difficult to meet the practical application. The main reason is that although polylactic acid is a crystalline polymer, it is difficult to fully crystallize in the actual molding process due to the slow crystallization rate. For this reason, a lot of research has been carried out on improving the crystallization rate of polylactic acid at home and abroad. Commonly used methods include adding nucleating agents and adding plasticizers. [0003] Nucleating agent is a k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08L71/08C08K5/21C08K5/11
Inventor 吴林波徐昱韬
Owner ZHEJIANG UNIV
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