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Preparing method of tetraphenylphosphonium phenolate

A technology of tetraphenylphenol and tetraphenylphosphine bromide, which is applied in the field of preparation of tetraphenylphenol phosphonium salt, can solve the problems of isopropanol, large amount of phenol, and difficulty in stratification, so as to improve reaction efficiency and Yield, reduction of technological process, and reduction of three wastes

Active Publication Date: 2019-09-24
KENTE CATALYSTS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. After the first layering, after adding deionized water, the organic phase is a solid-liquid mixture, and the water layer needs to be heated up to keep the separated water layer (the low-temperature crystallization is precipitated in advance, and it is difficult to layer), and the solid still needs isopropanol after suction filtration washing; many operating procedures are not conducive to industrial production;
[0005] 2. Isobutanol has a solubility of about 10% in water, and its boiling point is close, which is not conducive to separation
[0006] 3. The amount of phenol is too large, at least 5 times the amount

Method used

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  • Preparing method of tetraphenylphosphonium phenolate
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  • Preparing method of tetraphenylphosphonium phenolate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 28.2g of phenol, 69.5g of methanol, 36g of tetraphenylphosphine bromide, and 84g of pure water, and start stirring until all of them are dissolved, then add 8.7g of sodium hydroxide (50% aqueous solution) dropwise at a temperature of 20-25°C, After the dropwise addition, when the temperature is stable, raise the temperature to 45°C and stir for 80 minutes, cool to 20-22°C, pour out and filter with suction to obtain 74.5g of wet product and 140.5g of mother liquor.

[0030] The wet product was soaked and washed twice with 59.4g and 71g of pure water to obtain 58.3g of wet product and 30.9g of dry product (83.2% yield);

[0031] The mother liquor was supplemented with 13g of methanol, 36.0g of tetraphenylphosphine bromide, and 24.2g of phenol. After stirring and dissolving, 7.6g of sodium hydroxide (50% aqueous solution) was added dropwise at 20-25°C, and stirred at 45°C for 90min to obtain the second Batch product 36.6g;

[0032] The mother liquor was supplemented w...

Embodiment 2

[0035] The preparation method is the same as in Example 1, except that the amount of methanol is adjusted and its influence on the reaction is tested, as shown in Table 1.

[0036] Table 1

[0037]

[0038] As shown in table 1: the amount of methanol has a greater impact on the reaction, and the increase of methanol will reduce the yield of a single batch of products, but the residue can be applied mechanically in the mother liquor; the total yield after solvent recycling three times can reach 99.1%, Tetraphenylphosphine bromide can basically achieve quantitative conversion after four reactions.

Embodiment 3

[0040] The preparation method is the same as that of Example 1, the difference is that the reaction temperature and the recovery time are adjusted, and their influence on the reaction is tested, as shown in Table 2.

[0041] Table 2

[0042] serial number temperature reflex Response time / minute yield Example 3-1 20 70 81.6 Example 3-2 20 90 78.5 Example 3-3 22 90 79.4 Example 3-4 23 90 78.5 Example 3-5 25 90 79.5

[0043] As shown in Table 2, when the reaction temperature is controlled between 20-25°C, the yield deviation is small, and according to the test results, the reaction can be completed within 1h20min; when the temperature is ≥45°C, the color of the product will deepen;

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Abstract

The invention discloses a preparing method of tetraphenylphosphonium phenolate. The preparing method is characterized in that tetraphenylphosphonium bromide and phenol are added into a methanol solvent, wherein the mole ratio of the tetraphenylphosphonium bromide to the phenol is 1:(3-4); stirring is conducted until the materials are completely dissolved, then a sodium hydroxide aqueous solution is dropwise added at 20-25 DEG C, after dropwise adding is finished and the temperature is stable, the temperature is increased to 45 DEG C for 70-90 minutes of stirring, cooling is conducted to 20-22 DEG C, the materials are poured out, then suction filtration is conducted to obtain a wet product and a mother liquor, the wet product is soaked and washed twice with pure water, and then the dry product tetraphenylphosphonium phenolate is obtained. According to the preparing method, after the cheap and common solvent methanol is adopted for replacing isobutanol, secondary rinsing of isopropanol is not needed, and even if methanol and water are evaporated after the mother liquor is utilized multiple times, a mixture of the methanol and water can continue to be used multiple times; the mixed solvent of methanol and water is utilized, the crystallization time is short, few unreacted raw materials can be removed through centrifugation, the raw materials are put at the next batch to continue the reaction.

Description

Technical field: [0001] The invention discloses a preparation method of tetraphenylphenol phosphonium salt, belonging to the technical field of chemical synthesis. Background technique: [0002] As an important chemical raw material, tetraphenylphenol phosphine salt is mainly used as a transesterification catalyst, especially for the preparation of thermoplastic polycarbonate without using a solvent. [0003] At present, the preparation method of tetraphenylphenol phosphonium salt mainly adopts tetraphenylphosphonium bromide and phenol as raw materials, takes isopropanol as solvent, and uses ferric bromide, copper sulfate, etc. as catalysts to synthesize it, such as publication number In the literature of CN109942628A: "Take tetraphenylphosphine bromide, phenol and deionized water, add them to the reaction kettle, stir evenly, heat to 20-25 ° C, quickly add the sodium hydroxide solution with a mass percentage concentration of 48%, Adjust the pH value of the mixed solution t...

Claims

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Application Information

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IPC IPC(8): C07F9/54C07C39/04C07C37/00
CPCC07C37/00C07C39/04C07F9/5442
Inventor 李青山王新伟施旭升董柱永吴尖平
Owner KENTE CATALYSTS INC
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