Preparation and application of granular aluminum alkyl hypophosphite

A technology of aluminum alkyl phosphinate and alkyl phosphinic acid is applied in the field of granular organic aluminum phosphinate and its preparation, and can solve the problems of high price of nano metal oxides, affecting the purity of target products, and being unfavorable for industrialized production. , to achieve the effect of solving the problem of blanking, conducive to recycling and less by-products

Inactive Publication Date: 2018-02-02
JINAN TAIXING FINE CHEM
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] In the US300516 patent, a method for preparing aluminum alkyl phosphinate is reported, using peroxide as a free radical initiator to catalyze the addition reaction of phosphinic acid and olefins to synthesize the target product. The alkyl phosphinate prepared by this method Aluminum phosphinate exists in a powder state, the reaction needs to be carried out under high temperature and pressure, and other by-products will be produced, which will affect the purity of the target product
[0005] In the CN10372428A patent, a method for preparing aluminum alkylphosphinate is described, using sodium hypophosphite and olefins as raw materials, acetic acid as a solvent, and nanometer metal oxides as an initiator. Addition reaction occurs under certain conditions to synthesize the target Product, the aluminum alkyl phosphinate prepared by this method exists in a powder state, and acetic acid as a solvent has a high degree of corrosion to equipment, and the price of nano-metal oxides is relatively expensive, which is not conducive to industrial production
[0006] To sum up, in view of aluminum alkylphosphinate powder, there are difficulties in blanking and large dust in the process of processing, it is necessary to seek a production process with high conversion rate and safety factor, and the target product is easy to process. important practical significance

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  • Preparation and application of granular aluminum alkyl hypophosphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Concentrate 132g of 50% hypophosphorous acid solution by rotary evaporation under negative pressure, control the pressure at -0.09MPa, and increase the temperature from 35°C to 65°C at a rate of 15°C / h until the second The concentration of phosphoric acid reaches more than 80%;

[0028] 2) Put the above-obtained high-purity hypophosphorous acid in a 1L four-necked flask, add 12g of concentrated sulfuric acid as a dehydrating agent, 0.75g of tetrabutylammonium bromide as a phase transfer catalyst, and 100ml of chlorobenzene as a solvent;

[0029] 3) Weigh 150g of tert-butanol and 150ml of chlorobenzene to prepare a chlorobenzene solution of tert-butanol, add 2g of azobisisobutyronitrile as an initiator, keep stirring until it is completely dissolved, use a peristaltic pump at 15ml / min Add dropwise to the four-necked flask in step 2), and control the temperature to 70°C. After the solution is completely dropped, continue the reaction for 4 hours and then stop to obtain a ch...

Embodiment 2

[0033] 1) Concentrate 132g of 50% hypophosphorous acid solution by rotary evaporation under negative pressure, control the pressure at -0.09MPa, and increase the temperature from 35°C to 65°C at a rate of 10°C / h until the second The concentration of phosphoric acid reaches more than 80%;

[0034] 2) Put the high-purity hypophosphorous acid obtained above in a 1L four-necked flask, add 12g of concentrated sulfuric acid as a dehydrating agent, 0.75g of tetrabutylammonium chloride as a phase transfer catalyst, and 100ml of toluene as a solvent;

[0035] 3) Weigh 150g of tert-butanol and 180ml of toluene, prepare a toluene solution of tert-butanol, add 2g of di-tert-butyl peroxide as an initiator, and add the solution dropwise to step 2 with a peristaltic pump at a rate of 18ml / min In the four-necked flask, control the temperature to 117°C. After the solution is completely dripped, continue the reaction for 4 hours and then stop to obtain a toluene solution of organic phosphinic acid. ...

Embodiment 3

[0039] 1) Concentrate 132g of 50% hypophosphorous acid solution by rotary evaporation under negative pressure, control the pressure at -0.09MPa, and increase the temperature from 35°C to 65°C at a rate of 8°C / h until the second The concentration of phosphoric acid reaches more than 80%;

[0040] 2) Put the high-purity hypophosphorous acid obtained above in a 1L four-necked flask, add 12g of concentrated sulfuric acid as a dehydrating agent, 0.75g of tetrabutylammonium hydrogen sulfate as a phase transfer catalyst, and 100mL of toluene as a solvent;

[0041] 3) Weigh 150g of tert-butanol and 180mL of toluene, prepare a chlorobenzene solution of tert-butanol, add 2g of azobisisoheptonitrile as an initiator, and add the solution dropwise to step 2 with a peristaltic pump at a rate of 20ml / min In the four-necked flask in ), control the temperature to 60°C, after the solution is completely dripped, continue the reaction for 4 hours and then stop to obtain the toluene solution of organic...

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Abstract

The invention discloses a preparation method and application of a granular aluminum alkyl hypophosphite, and the preparation method is as follows: radical initiator catalyzed addition reaction in an organic solvent as a solvent of hypophosphorous acid and an alcohol as raw materials for synthesis of alkyl phosphinic acid, and double decomposition reaction of the alkyl phosphinic acid with an aluminum salt in the presence of an organic solvent to obtain the granular aluminum alkyl hypophosphite. The granular aluminum alkyl hypophosphite is applied to flame retardance of polyamide, polyester, thermosetting plastics and elastomers such as PA6, PA66, PBT, PET, PU and EVA, and shows excellent flame retardancy. The granular aluminum alkyl hypophosphite can solve the problems of material discharging difficulty and lot of dust in the processing process, the alcohol replaces an olefin as a raw material, reaction yield and safety coefficient are high, byproducts are few, because the organic solvent and water are immiscible, the difficulty of post separation is reduced, and solvent recovery is easier.

Description

Technical field [0001] The invention relates to the field of organic synthesis, in particular to a granular organic aluminum phosphinate and a preparation method thereof. Background technique [0002] Alkyl phosphinate flame retardant is a kind of environmentally friendly non-halogen organophosphorus flame retardant with good hydrophobicity. Due to its relatively high phosphorus content and unique P-H bond, it has excellent flame retardant properties in a variety of thermoplastics and thermosetting plastics. Clariant's OP series is the main representative of aluminum alkyl phosphinates on the market. Alkyl aluminum hypophosphites currently sold on the market are all in the form of powder, but due to their low density, there will be a problem of difficulty in blanking during processing, and more dust will be generated. [0003] The existing method for preparing aluminum alkylphosphinate is mainly a free radical addition method, that is, hypophosphorous acid or its alkali metal sal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08L77/02C08L77/06C08L67/02C08K5/5313
CPCC07F9/30C08K5/5313C08L2201/02C08L77/02C08L77/06C08L67/02
Inventor 周生刚杜庆田刘彦余徐亮王鲁静索伟游永胜王艳辉肖学文
Owner JINAN TAIXING FINE CHEM
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