A clean preparation method of submicron calcium terephthalate

A technology of calcium terephthalate and ammonium terephthalate, which is applied in the chemical field, can solve the problems of environmental pollution, lack, and no clear particle size of calcium terephthalate, and achieve a high degree of cleanliness and reduced environmental protection costs , the effect of huge potential economic benefits

Active Publication Date: 2017-09-19
JIANGSU ATE DONGTAI NEW MATERIALS TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Calcium terephthalate reported in Chinese patents CN 103173845B, CN102583813B and CN104292100B are obtained by reacting sodium terephthalate solution with soluble calcium compound. The method is simple and easy, but the filtrate after separating calcium terephthalate is sodium Salt solution cannot be recycled in this system, and direct discharge will pollute the environment
The calcium terephthalate reported in the Chinese patent CN103820860A is obtained by heating the mixture of terephthalic acid and calcium hydroxide to 95°C and reacting for 1 hour under ultrasonic conditions. diameter, but it can be seen from the attached figure that its particles are tens of microns, belonging to micron-scale products
[0004] At present, there is a lack of a clean preparation method of submicron calcium terephthalate, not only does the whole preparation process produce no "three wastes", but also the obtained product can improve the comprehensive performance of polymer materials

Method used

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  • A clean preparation method of submicron calcium terephthalate
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  • A clean preparation method of submicron calcium terephthalate

Examples

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Embodiment 1

[0023] A clean preparation method of submicron calcium terephthalate of the present invention comprises the following steps: introducing the calcium hydroxide slurry from the upper end of the jet reactor with a porous nozzle, and pre-adding the parabenzene The ammonium diformate solution is introduced from the side of the jet reactor through a high-speed centrifugal atomizer. After the two are fully mixed in the mixing chamber of the jet reactor, they leave the jet reactor through the diffusion chamber and then enter the closed tank reactor. , heating the material to the specified temperature while stirring, continue to mix and react for a certain period of time, and finally separate, wash, and dry at a temperature not higher than 100°C to obtain calcium terephthalate trihydrate.

[0024] The calcium hydroxide slurry is obtained by dissolving and dispersing solid calcium hydroxide in hot water at 40° C., and the mass percent concentration of the calcium hydroxide slurry is 5%. ...

Embodiment 2

[0034] The difference between embodiment 2 and embodiment 1 is:

[0035] 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%.

[0036] In the ammonium terephthalate solution added with sodium hexametaphosphate, the mass percent concentration of ammonium terephthalate 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%. The quality of sodium hexametaphosphate is 3.5% of the quality of generated calcium terephthalate.

[0037] The specified temperature is 80°C.

[0038] The specified time is 24 hours.

[0039] The reaction molar ratio of described calcium hydroxide and ammonium terephthalate is 1.1: 1.

[0040] Figure 4 The particle size distribution curv...

Embodiment 3

[0042] The difference between embodiment 3 and embodiment 1 is:

[0043]The calcium hydroxide slurry is obtained by dissolving and dispersing solid calcium hydroxide in hot water at 75° C., and the mass percent concentration of the calcium hydroxide slurry is 20%.

[0044] In the ammonium terephthalate solution added with sodium polyacrylate, the mass percent concentration of ammonium terephthalate is 9%. 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 9%. The quality of sodium polyacrylate is 2% of the quality of generated calcium terephthalate.

[0045] The specified temperature is 70°C.

[0046] Said certain time is 12h.

[0047] The reaction molar ratio of described calcium hydroxide and ammonium terephthalate is 1.0: 1.

[0048] Figure 4 The particle size distribution curve in shows that the m...

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Abstract

The invention discloses a clean preparation method of submicron calcium terephthalate. The preparation method comprises the following steps: a calcium hydroxide slurry with a multihole nozzle is introduced from the upper end, and an ammonium terephthalate solution with a dispersion modifier is introduced through the side surface of a high-speed centrifugal atomizer; the calcium hydroxide slurry and ammonium terephthalate solution are sufficiently mixed in a mixing chamber of a jet reactor, and enter a closed tank reactor via a diffuser chamber; and the materials are heated to the specified temperature while stirring to continue react for some time, thereby obtaining the calcium terephthalate. The method is green and environment-friendly, has high clean degree, and does not generate three wastes in the preparation process; and the obtained product is submicron particles. In the submicron calcium terephthalate preparation process, the separated ammonia water can continue dissolving terephthalic acid to enter the next circulation, or after ammonia gas is recovered by an ammonia evaporation technique, the residual water can be recycled, so the whole process does not generate three wastes and belongs to clean production.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a clean preparation method for submicron calcium terephthalate. Background technique [0002] Calcium terephthalate is a metal salt of organic acid. Its molecular structure contains organic skeleton and ionic bonds. It has good compatibility with polar polymer materials such as polyvinyl chloride, nylon and polyester. The development of calcium terephthalate with different crystal structures and its application are the focus of research in the industry. For example, submicron near-spherical calcium terephthalate can improve the toughness of polymer materials, and whisker-shaped calcium terephthalate can Improve the strength of polymer composite materials. [0003] Calcium terephthalate reported in Chinese patents CN 103173845B, CN102583813B and CN104292100B are obtained by reacting sodium terephthalate solution with soluble calcium compound. The method is simple and easy, but the filtra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/28C07C51/41
CPCC07C51/412C07C63/28
Inventor 张莉娜宋兴福孙玉柱蒋丽方春平
Owner JIANGSU ATE DONGTAI NEW MATERIALS TECH
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