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Cellulose long chain fatty acid phthalate and synthesis preparation method therefor

A technology of phthalates and long-chain fatty acids, which is applied in the field of new cellulose esters and their synthesis and preparation, can solve problems such as no synthetic process methods, avoid potential harm to the human body, overcome dependence on plasticizers, The effect of process condition moderation

Active Publication Date: 2016-01-13
EASTERN LIAONING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in the prior art, there is no relevant bibliographic record of the synthesis process method of introducing long-chain fat by cellulose acetate phthalate

Method used

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  • Cellulose long chain fatty acid phthalate and synthesis preparation method therefor
  • Cellulose long chain fatty acid phthalate and synthesis preparation method therefor
  • Cellulose long chain fatty acid phthalate and synthesis preparation method therefor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Synthesis of cellulose caprylic acid phthalate with homogeneous cellulose DMAc / LiCl solution:

[0020] Step 1, the synthesis of cellulose octanoate:

[0021] Put 50 g of cellulose DMAc / LiCl solution with a mass concentration of 2% into a 100 ml three-necked flask, and start the stirring device; the molar ratio of cellulose anhydroglucose unit (AGU) to octanoyl chloride n(AGU):n(octanoyl chloride ) at a ratio of 1:2, add a certain amount of octanoyl chloride, and then add 5ml of acid-binding agent pyridine to reduce the degradation effect of hydrochloric acid generated by the reaction on cellulose, react at a temperature of 50°C for 12 hours, and then cool to room temperature for use ;

[0022] Step 2: Add 2 g of phthalic anhydride and 5 ml of catalyst triethylamine to the system after the reaction in Step 1, stir and react for 30 minutes at room temperature, and then use an aqueous solution with a concentration of 35% hydrochloric acid and water at a volume ratio of 1:...

Embodiment 2

[0025] Synthesis of cellulose nonanoic acid phthalate with homogeneous cellulose DMAc / LiCl solution;

[0026] Step 1: Synthetic reaction of cellulose nonanoate

[0027] Add 50 g of cellulose DMAc / LiCl solution with a mass concentration of 2% to a 100 ml three-necked bottle, and use the molar ratio of cellulose anhydroglucose unit: nonanoic acid: p-toluenesulfonyl chloride n(AGU):n(nonanoic acid): n (p-toluenesulfonyl chloride) is 1:4:4. Add nonanoic acid and p-toluenesulfonyl chloride. The p-toluenesulfonyl chloride is a solution dissolved in 5ml of DMAc. Add 6ml of pyridine to reduce and weaken the hydrochloric acid produced in the reaction. For the effect on the degradation of cellulose, stir and react at 50°C for 12 hours, then cool to room temperature and set aside;

[0028] Step 2: Add 2 g of phthalic anhydride and 5 ml of catalyst triethylamine to the system after the reaction in Step 1, stir and react for 30 minutes at room temperature, and then use an aqueous solution...

Embodiment 3

[0031] Synthesis of cellulose capric acid phthalate with homogeneous cellulose DMAc / LiCl solution:

[0032] Step 1: Synthesis of cellulose caprate:

[0033]Add 50 g of cellulose DMAc / LiCl solution with a mass concentration of 2% into a 100 ml three-necked flask, turn on the stirring device, and the molar ratio of the anhydroglucose unit of cellulose: capric acid: p-toluenesulfonyl chloride n(AGU):n( Decanoic acid): n (p-toluenesulfonyl chloride) is 1:4:4. Add capric acid and p-toluenesulfonyl chloride, wherein p-toluenesulfonyl chloride is a solution dissolved in 5ml of DMAc, and then add 6ml of acid-binding agent pyridine to reduce, To weaken the effect of hydrochloric acid produced in the reaction on the degradation of cellulose, raise the temperature to 50°C and maintain the reaction for 12 hours, then cool down to room temperature, pour it into distilled water to precipitate, filter with suction, and wash the filtered product with ethanol at 50°C for two to three times , ...

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Abstract

The present invention provides a cellulose long chain fatty acid phthalate and a synthesis preparation method therefor. The cellulose long chain fatty acid phthalate is prepared by carrying out reaction on a fatty acylating agent and a homogeneous cellulose DMAc / LiCl solution at 50 DEG C to 80 DEG C for 2-12 hours to prepare a cellulose long chain fatty acid ester; and then carrying out reaction on the cellulose long chain fatty acid ester and phthalic anhydride and a catalyst at room temperature, and washing and drying the product. Presence of long chain fatty ester groups in the cellulose long chain fatty acid phthalate greatly improves the workability of cellulose acetate phthalate (CAP) and overcomes the dependency of the existing cellulose acetate phthalate (CAP) on plasticizers in terms of workability. The technical scheme of the present invention further has the technical advantages of mild process condition, easy implementation, no to-be-separated intermediates during the reaction, short preparation time, recyclable cellulose DMAc / LiCl solution and the like.

Description

technical field [0001] The patent application of the present invention relates to fiber derivatives and their synthesis and preparation methods, in particular to a novel cellulose ester and its synthesis and preparation methods. Background technique [0002] Cellulose is the most widely distributed in nature, and its derivatives are widely used in the fields of textile, light industry, chemical industry, petroleum, medicine, energy and biotechnology. Among them, cellulose acetate is an important cellulose ester, also known as cellulose acetate. Its technology has been industrialized, and it is modified and applied again. For example, many cellulose derivatives are prepared based on cellulose acetate. Such as cellulose acetate phthalate (CAP). In Jia Xinyan's master's thesis "Synthesis and Properties of Cellulose Acetate Derivatives", the synthesis technology of cellulose acetate phthalate (CAP) is described in detail. The synthesis scheme is: use acetic acid as solvent and ...

Claims

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Application Information

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IPC IPC(8): C08B3/16
Inventor 于艳黄凤远刘波吴晓杰
Owner EASTERN LIAONING UNIV
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