Method for preparing bisphenol phosphate hydroxyl aluminum salt nucleating agent

Abstract

A method for preparing a bisphenol phosphate hydroxyl aluminum salt nucleating agent is provided, which adopts organic aluminum alcoholate as raw materials to prepare bisphenol phosphate hydroxyl aluminum salt. In prior art, a neutralization reaction of bisphenol phosphate and sodium hydroxide is firstly performed, so as to prepare bisphenol phosphate sodium salt; then a double decomposition reaction of sodium salt and inorganic aluminum salt is performed to prepare the bisphenol phosphate hydroxyl aluminum salt. The present invention combines the two-step reaction in prior art into the one-step reaction of phosphate and organic aluminum alcoholate for synthesizing the bisphenol phosphate hydroxyl aluminum salt, thereby simplifying the production process, improving the production efficiency, shortening the reaction time, and improving the product quality. Moreover, during the production process of the preparation method provided by the present invention, no brine waste is generated, so that the production process is environment-friendly.

Claims

1. A method for preparing a bisphenol phosphate hydroxyl aluminum salt nucleating agent, comprising steps of: (1) adding bisphenol phosphate and alkyl aluminum alcoholate into an organic solvent; reacting at a certain temperature, and obtaining an intermediate; and (2) adding water into the intermediate obtained through the step (1), then hydrolyzing, and distilling, so as to remove by-product alcohols and the organic solvent; filtering, drying, and finally obtaining the bisphenol phosphate hydroxyl aluminum salt nucleating agent.

2. The method, as recited in claim 1, wherein: the bisphenol phosphate hydroxyl aluminum salt nucleating agent is bis [2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate] hydroxyl aluminum salt, and a structural formula thereof is: ##STR00011## .

3. The method, as recited in claim 1, wherein: the bisphenol phosphate is 2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate, and a structural formula thereof is: ##STR00012## .

4. The method, as recited in claim 1, wherein: the aluminum alcoholate (Al(OR).sub.3) is low-carbon aluminum alcoholate containing 1-4 carbon atoms.

5. The method, as recited in claim 4, wherein: the intermediate is bis [2,2′-methylene-bis(4,6-di-tert-butylphenyl)phosphate] alcohol group aluminum salt, and a structural formula thereof is: ##STR00013## .

6. The method, as recited in claim 5, wherein: an alcohol group in the alcohol group aluminum salt is low-carbon alcohol containing 1-4 carbon atoms, corresponding to the aluminum alcoholate (Al(OR).sub.3).

7. The method, as recited in claim 1, wherein: in the step (1), an addition amount of the alkyl aluminum alcoholate is 0.95-1.05 times a theoretical amount; an amount of the organic solvent is 1.5-6 times a weight of the bisphenol phosphate.

8. The method, as recited in claim 1, wherein: the organic solvent is alkane, cycloalkane, benzene, methylbenzene, dimethylbenzene, or chloroalkane.

9. The method, as recited in claim 1, wherein the certain temperature in the step (1) is 25° C.-140° C.

10. The method, as recited in claim 9, wherein the certain temperature is 70° C.-110° C.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0020] The FIGURE shows FT-IR spectrums of bisphenol phosphate hydroxyl aluminum salt nucleating agent.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

Contrast Example

[0021] Adding 3.34 g sodium hydroxide and 100 ml water into a reaction flask; stirring, and adding 36 g bisphenol phosphate; heating to 80° C., and keeping reaction for 2 hours; performing suction filtration, drying, and obtaining the bisphenol phosphate sodium salt; adding the bisphenol phosphate sodium salt into 170 ml mixed solution of ethyl alcohol and water; rising a temperature to about 60° C.; after the bisphenol phosphate sodium salt is completely dissolved, dripping a mixed solution of 8.4 g aluminum trichloride and 10 ml water into a reaction kettle, and reacting for two hours; adding 1.56 g caustic soda flakes into the reaction kettle, and reacting for half hour; performing suction filtration, drying, and obtaining bisphenol phosphate hydroxyl aluminum salt.

Example of Present Invention

[0022] Adding 12 g bisphenol phosphate, 2.65 g aluminum isopropoxide and 60 ml methylbenzene into a reaction flask; stirring, slowly heating, and distilling by-products; after reacting completely, adding water, distilling, and recycling the methylbenzene; after distillation is completed, cooling, performing suction filtration, drying, and obtaining the product of bisphenol phosphate hydroxyl aluminum salt.

Product Testing

[0023] 1. Element analysis

TABLE-US-00001 Product Phosphorus content (%) Aluminum content (%) Contrast example 5.91 2.41 Example of present invention 6.23 2.68 Theoretical value 6.17 2.69

[0024] The element analysis conclusion is described as follows. The contrast example prepares the product with the conventional method; in comparison, the example prepares the product with the method provided by the present invention, and the element analysis result thereof is closer to the theoretical value.

[0025] 2. Infrared analysis

[0026] The figure shows FT-IR spectrums of bisphenol phosphate hydroxyl aluminum salt nucleating agent. The infrared peak positions of 1100 cm.sup.-1 and 880 cm.sup.-1 are the characteristic peaks of P-O-M (M for metal). When the valence state of M changed from univalent to multivalent substitution, the peak type will be divided into two. The peak type of the contrast example is single peak at 1100 cm.sup.-1, and the double peak at 880 cm.sup.-1 is not obvious, while the example of the present invention is double peak. Therefore, it can be judged that the response degree of the contrast example is lower.