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Nucleating agent and preparation method thereof

A technology of nucleating agent and acylating agent, applied in the field of nucleating agent and its preparation, can solve the problems of poor compatibility of polylactic acid matrix, reduction of reagent addition, insufficient formation of crystal nuclei, etc.

Active Publication Date: 2014-04-02
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, it is reported that the interaction between bisamide compounds and polylactic acid molecules can be used to improve the crystallization nucleation ability of polylactic acid, so as to obtain a modified polylactic acid with fast crystallization rate and low production cost, but such compounds are based on One or two of the substituents such as alkyl, hydroxyl, nitro, amino, and alkoxy are end groups, which have poor compatibility with the polylactic acid matrix, resulting in reduced reagent addition, insufficient crystal nucleus formation, and improved Crystallization nucleation ability is not obvious, there are still technical shortcomings
[0005] With the continuous expansion of PLA application fields, people's requirements for nucleating agents are also increasing, and the existing nucleating agents are gradually difficult to meet all application needs. Therefore, it is important to design and synthesize new and efficient PLA nucleating agents. Practical significance

Method used

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  • Nucleating agent and preparation method thereof
  • Nucleating agent and preparation method thereof
  • Nucleating agent and preparation method thereof

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preparation example Construction

[0034] The present invention also provides a preparation method of the nucleating agent represented by the above formula (I), comprising the following steps:

[0035] Mixing 5-sulfoisophthalic acid with an acylating agent, heating for acylation reaction, and then adding benzyl alcohol for alcoholysis reaction to obtain a nucleating agent represented by formula (I);

[0036] Or mix 5-sulfoisophthalic acid with an acylating agent to carry out acylation reaction, then add benzyl alcohol to carry out alcoholysis reaction, then add M metal or a compound containing M to carry out a salt-forming reaction to obtain the formula ( I) the indicated nucleating agent;

[0037]

[0038] Wherein, M is H, an alkali metal atom or an alkaline earth metal atom, and n is the valence of M.

[0039] The present invention has no special limitation on the sources of all raw materials, which can be commercially available.

[0040] The 5-sulfoisophthalic acid is preferably prepared according to th...

Embodiment 1

[0065] 1.1 Add 10g of isophthalic acid into a 150ml three-necked round-bottomed flask equipped with a reflux condenser, then add 20ml of 20% oleum, and heat the oil bath to 185°C for 6 hours under stirring conditions. After the reaction, remove the oil The bath was cooled to room temperature, the reaction system was diluted with distilled water, and fully cooled to precipitate 5-sulfoisophthalic acid to obtain 5-sulfoisophthalic acid.

[0066] 1.2 Add the 5-sulfoisophthalic acid obtained in 1.1 to a 250ml round-bottomed flask, add 40ml of thionyl chloride, and heat under reflux at 80°C for 5 hours. After the reaction, remove the remaining thionyl chloride and turn the reaction flask Cool in an ice-water bath, slowly add 30ml of benzyl alcohol dropwise, and carry out alcoholysis reaction. During the alcoholysis reaction, control the reaction temperature at 0°C to 30°C. After reacting for 5 hours, separate and purify to obtain the formula (I) in which M is H The nucleating agent...

Embodiment 2

[0071] The dibenzyl isophthalate obtained in Example 1 is mixed with 40% potassium carbonate aqueous solution, and a salt-forming reaction is carried out until the pH value is neutral, separated by filtration, and M is shown in formula (I) of K. The nucleating agent is an aromatic sulfonic acid potassium salt compound, the structure of which is shown in formula (III).

[0072]

[0073] Utilize infrared spectrometer to analyze the aromatic sulfonic acid potassium salt compound obtained in embodiment 2, obtain its infrared spectrogram, as figure 1 shown. Depend on figure 1 It can be seen that 3044cm -1 The C-H stretching vibration peak of the benzene ring appears at 2942cm -1 and 2874cm -1 methylene-CH 2 The characteristic peak of -, 1721cm -1 The characteristic peak of ester C=O appears at 1611cm -1 、1508cm -1 and 1449cm -1 The characteristic vibration peak of the benzene ring skeleton appears at 1185cm -1 is the characteristic peak of the sulfo group.

[0074] Th...

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Abstract

The invention provides a nucleating agent and a preparation method thereof. The nucleating agent is represented by a formula (I) as described in the specification; and in the formula, M is H, an alkali metal atom or an alkaline earth metal atom. Compared with a conventional nucleating agent, the nucleating agent provided by the invention has the following advantages: the nucleating agent has a highly molecularly symmetric structure, which is beneficial for induction of crystallization; and the nucleating agent contains three phenyl ring structures, and an increase of phenyl rings in a molecular structure is beneficial for promotion of crystallization and improvement of the degree of crystallization.

Description

technical field [0001] The invention belongs to the technical field of resin materials, and in particular relates to a nucleating agent and a preparation method thereof. Background technique [0002] Polylactic acid (PLA), as a synthetic thermoplastic aliphatic polyester, has attracted much attention in recent years. The raw materials for the synthesis of PLA are drawn from biological resources. It is a kind of renewable biological resources as raw materials. It is prepared by chemical synthesis and has renewability. At the same time, PLA also has excellent biodegradability and biocompatibility. eventually decomposed into CO 2 and H 2 O, so it is pollution-free, and it is an environmentally friendly material in the true sense; not only that, many performance indicators of PLA are similar to general-purpose plastics such as polyethylene, polypropylene, and polystyrene, and it has good mechanical properties, non-toxicity, and relatively high density. Low temperature, easy t...

Claims

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Application Information

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IPC IPC(8): C08L67/04C08K5/42C08K5/41C07C309/29C07C303/32
Inventor 孙志强张涵庞烜庄秀丽边新超陈文啟陈学思
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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