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Synthesis method for biologically based transparent semi-aromatic poly-amide material

A technology of semi-aromatic polyamide and synthesis method, which is applied in the field of bio-based transparent semi-aromatic polyamide material synthesis, can solve the problems of importing transparent polyamide and failing to successfully develop transparent polyamide, etc., and achieves high environmental protection and economical and practical value. , the effect of excellent transparency and good thermal stability

Inactive Publication Date: 2014-10-15
GUANGDONG WAYLAM ENG PLASTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] At present, the annual consumption of transparent polyamides in China has reached more than 2,000 tons, but since the aliphatic diamines and dibasic acid monomers used to synthesize transparent polyamides have not yet been industrialized in China, transparent polyamides have not been successfully developed so far. All the required products need to be imported from abroad, and the price is as high as 30,000 yuan / ton. In order to meet the needs of transparent polyamides at home and abroad and solve the problem of transparent polyamides’ long-term dependence on imports, the research on bio-based transparent polyamides has a very important role. important practical significance

Method used

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  • Synthesis method for biologically based transparent semi-aromatic poly-amide material

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Experimental program
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Embodiment 1

[0027] Put 1Kg of lignin in 7L of toluene / ethanol (volume ratio=1:2) mixed solution, stir for 6h at normal temperature and pressure, then filter, wash 2-3 times with 95% ethanol solution, dry, Obtain relatively pure lignin. Put purified 0.5mol of purified lignin and 1mol of terephthalic anhydride in 7L of glacial acetic acid at a molar ratio of 1:2, add concentrated sulfuric acid (0.5-1wt%) as a catalyst, and react under reflux conditions 8h, after the reaction, filter and dry to obtain acetylated lignin.

[0028] Weigh 2mol of the above-mentioned acetylated lignin, 2mol of terephthalic acid, 4mol of 1,10-decanediamine in 15L of dimethylformamide organic solvent, and react at 105°C for 5 hours under stirring conditions. The reaction is complete After cooling and filtering, a relatively pure amide salt is obtained.

[0029] Put 2 mol of the amide salt prepared above, 50 mol of deionized water, benzoic acid (0.6 mol), and sodium hypochlorite (0.08 mol) in a reaction kettle with a ...

Embodiment 2

[0031] The lignin was acetylated in the same way as in Example 1.

[0032] Weigh 2mol of the above-mentioned acetylated lignin, 2mol of terephthalic acid, 4mol of 1,11-aminoundecane in 15L of dimethylformamide organic solvent, and react at 105°C for 5 hours under stirring conditions. Cool and filter after completion to obtain a purer amide salt.

[0033] Put 2 mol of the amide salt prepared above, 50 mol of deionized water, benzoic acid (0.6 mol), and sodium hypochlorite (0.08 mol) in a reaction kettle with a temperature control of 230°C and stirring for 3 hours in a high-purity nitrogen atmosphere. After the reaction is completed, the temperature is increased to 260°C, the pressure is increased to 3MPa, and the reaction is 3 hours. After the reaction is completed, the pressure is reduced to normal pressure within 1 hour, and the reaction is 1 hour to discharge, cool, and pellet to prepare the organism Base transparent semi-aromatic polyamide material.

[0034] Table 1 is the pe...

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Abstract

The invention relates to a synthesis method for a biologically based transparent semi-aromatic poly-amide material, and belongs to the field of polyamide synthesis. The synthesis method is characterized by comprising the following steps: purifying a biologically based lignose material and performing acetylation treatment; conducting reaction for acetylated lignose material, aromatic dicarboxylic acid, aliphatic diamine of 6-12 carbon atoms in an organic solvent to prepare high purity salt; placing the salt obtained through the reaction, deionized water and polymeric additives into a high pressure reaction kettle, and performing prepolymerization under the condition of high-purity inert gas; after the prepolymerization, increasing temperature and pressure to further performing a polymerization reaction to obtain the novel biologically based transparent semi-aromatic poly-amide material. The novel biologically based transparent semi-aromatic poly-amide material has excellent transparency, heat resistance, electric insulativity and aging resistance, is high in strength, non-toxic, odor free and corrosion resistant, and can be widely applied to automotive industry, medicine devices, optical instruments, measure instruments, food packages, physical goods and the like.

Description

Technical field [0001] The present invention relates to the field of synthesis of a new type of transparent polyamide, in particular to a method for synthesizing a bio-based transparent semi-aromatic polyamide material, in particular to a lignin and aromatic type two through acetylation treatment. A new type of bio-based semi-aromatic polyamide material synthesized in a reactor with carboxylic acid and aliphatic diamine under the action of polymerization assistants. Background technique [0002] Polyamide, commonly known as nylon (PA), refers to a polymer with amide group (-CONH-) repeating structural units on the polymer chain. It was developed and industrialized by WH Carothers of the Central Research Institute of DuPont in the 1930s. , Has a history of more than 60 years. In the early stage of production, it was mainly used for spinning, and it was only used as an engineering plastic in the early 1950s. Because of its high mechanical strength, good impact toughness, exc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/28C08G69/26C08H7/00
Inventor 阳瑞皮正亮薛鹏葛嘉宝郭建强
Owner GUANGDONG WAYLAM ENG PLASTICS