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Preparation method and application of anhydrous calcium terephthalate whiskers

A technology of calcium terephthalate and ammonium terephthalate, applied in the field of chemistry, can solve the problems of obvious reinforcing properties of polymer materials, lack of terephthalic acid whiskers, and cannot be recycled, and achieves a remarkable reinforcing effect. , huge potential economic benefits, the effect of reducing environmental protection costs

Active Publication Date: 2016-11-16
JIANGSU ATE DONGTAI NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of whisker-shaped calcium terephthalate has been reported in Chinese patent CN 103173845B and CN102583813B, all is to add thick terephthalic acid to caustic soda solution and dissolve, adjust pH, add polyethylene glycol nonionic surfactant, stir Mix well, then add soluble calcium salt, stir, and age for a certain period of time to obtain calcium terephthalate whiskers. This method is simple and easy, but the filtrate after separating the calcium terephthalate whiskers is a sodium salt solution. It cannot be recycled in this system, and direct discharge will pollute the environment
[0004] At present, there is a lack of a clean preparation process for terephthalic acid whiskers. Not only does the whole production process produce no three wastes, but the obtained whiskers have a significant reinforcing performance on polymer materials.

Method used

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  • Preparation method and application of anhydrous calcium terephthalate whiskers
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  • Preparation method and application of anhydrous calcium terephthalate whiskers

Examples

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Embodiment 1

[0020] A method for preparing anhydrous calcium terephthalate whiskers of the present invention comprises the following steps: the precursor obtained by reacting ammonium terephthalate solution and calcium hydroxide slurry is continued in an autoclave at 120°C After reacting for 2 hours, anhydrous calcium terephthalate whiskers were obtained. The obtained anhydrous calcium terephthalate whiskers can be added to polymer materials as a reinforcing agent to prepare composite materials with high strength and high modulus.

[0021] The preparation method of the precursor is to slowly add the calcium hydroxide slurry to the ammonium terephthalate solution under constant stirring, and then continue the reaction for 5 minutes.

[0022] The mass percent concentration of the ammonium terephthalate solution is 2%. The ammonium terephthalate solution is prepared by dissolving terephthalic acid in ammonia solution, or directly dissolving commercially available ammonium terephthalate solid...

Embodiment 2

[0031] The difference between Example 2 and Example 1 is that a method for preparing anhydrous calcium terephthalate whiskers of the present invention comprises the following steps: the precursor obtained by reacting ammonium terephthalate solution and calcium hydroxide slurry , continue the reaction in an autoclave at 140° C. for 4 hours to obtain anhydrous calcium terephthalate whiskers. The obtained anhydrous calcium terephthalate whiskers can be added to polymer materials as a reinforcing agent to prepare composite materials with high strength and high modulus.

[0032] The mass percent concentration of the ammonium terephthalate solution is 10%. The ammonium terephthalate solution is prepared by dissolving terephthalic acid in ammonia solution, or directly dissolving commercially available ammonium terephthalate solid in water, and its mass percent concentration is 10%.

[0033] The calcium hydroxide slurry is obtained by dissolving and dispersing solid calcium hydroxide...

Embodiment 3

[0036] The difference between Example 3 and Example 1 is that a method for preparing anhydrous calcium terephthalate whiskers of the present invention comprises the following steps: the precursor obtained by reacting ammonium terephthalate solution and calcium hydroxide slurry , continue the reaction in an autoclave at 150° C. for 6 h to obtain anhydrous calcium terephthalate whiskers.

[0037] The mass percent concentration of the ammonium terephthalate solution is 15%. The ammonium terephthalate solution is prepared by dissolving terephthalic acid in ammonia solution, or directly dissolving commercially available ammonium terephthalate solid in water, and its mass percent concentration is 15%.

[0038]The calcium hydroxide slurry is obtained by dissolving and dispersing solid calcium hydroxide in hot water at 90° C., and the mass percent concentration of the calcium hydroxide slurry is 25%.

[0039] The reaction molar ratio of the calcium hydroxide to the ammonium terephtha...

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Abstract

The invention discloses a preparation method and application of anhydrous calcium terephthalate whiskers. The preparation method of anhydrous calcium terephthalate whiskers includes the steps of subjecting ammonium terephthalate solution and calcium hydroxide slurry to reaction to obtain a precursor, and continuing the reaction at 120-150 DEG C in a high-pressure kettle for 1-6 h to obtain the anhydrous calcium terephthalate whiskers. The preparation method is green, low in cost and high in cleanliness level. The production process is free of three wastes, and the obtained anhydrous calcium terephthalate whiskers have large length-diameter ratio, high crystal strength and significant reinforcement effect. During the preparation of the calcium terephthalate whiskers from ammonium terephthalate and calcium hydroxide, isolated ammonia water may continue to dissolve terephthalic acid for next cycle or remaining water is also suitable for reuse after ammonia gas is recycled by means of ammonia steaming, and the whole process is free of three wastes and belongs to clean production.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a preparation method and application of anhydrous calcium terephthalate whiskers. Background technique [0002] Whiskers have a certain length-to-diameter ratio, generally the length-to-diameter ratio is greater than 10, and the cross-sectional area is less than 52×10 -5 cm 2 The single crystal fiber material has a fine diameter, almost no defects such as dislocations, cavities, impurities, and particle interfaces contained in common materials, and has complete crystallization and orderly arrangement, so its strength is close to the theoretical limit of atomic bonding. The strength of whiskers far exceeds that of ordinary fiber materials, and it is a reinforcing agent for new composite materials with excellent mechanical properties. At present, it is mainly used in the reinforcement of ceramic matrix composite materials, metal matrix composite materials and resin matrix composite mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/54C30B29/62C30B7/10
CPCC30B7/105C30B29/54C30B29/62
Inventor 张莉娜孙淑英宋兴福吴宇浩方春平
Owner JIANGSU ATE DONGTAI NEW MATERIALS TECH
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