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Preparation method and application of dialkyl phosphinate with high density and large diameter

A technology of dialkyl phosphinate and alkyl phosphinate, which is applied in the field of preparation of high density and large particle size dialkyl phosphinate, can solve the problem of low particle size of dialkyl phosphinate, Plastic particles are difficult to mix evenly, which is not conducive to resin molding processing, etc., to achieve the effect of easy feeding, small dust and easy packaging

Inactive Publication Date: 2013-05-15
ZHUHAI WANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Its main feature of the synthetic method of dialkylphosphinate disclosed in the above method is that alkylphosphinic acid is directly reacted with aqueous inorganic salt solution, and has the following defects: The dialkylphosphinate prepared by the above method has low particle size and low bulk density. When used as a flame retardant in plastic processing, it has the disadvantages of difficult feeding, large dust, difficult mixing with plastic particles, and poor processing performance.
[0007] In order to solve the above problems, the German patent DE 0241376A1 adopts the method of impact compaction to improve the vibration of dialkylphosphinate flame retardants to a certain extent Density, but this method is time-consuming and laborious and difficult to be accepted by people; German patent DE 0241375A1 improves the tap density of dialkylphosphinate flame retardants to a large extent through the melting method, but this method adds A large amount of wax and other auxiliary substances are not conducive to the molding process of the resin

Method used

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  • Preparation method and application of dialkyl phosphinate with high density and large diameter
  • Preparation method and application of dialkyl phosphinate with high density and large diameter
  • Preparation method and application of dialkyl phosphinate with high density and large diameter

Examples

Experimental program
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Effect test

Embodiment 1

[0040] (1) Synthesis of dialkylphosphinic acid and / or alkali metal salt of dialkylphosphinic acid

[0041] The dialkylphosphinic acid and / or the alkali metal salt of dialkylphosphinic acid used in the examples listed in the method of the present invention are all synthesized with reference to Chinese patent CN 201010613835.6.

[0042] (2) Preparation of aluminum diethylphosphinate

[0043] Add 2711g and 10mol of 45% diethylphosphinic acid aqueous solution into the reactor, add 3000g and 30mol of 40% NaOH aqueous solution into the reactor, stir and heat to 95°C, add 40% octadecadecanoic sulfuric acid Add 2780g and 1.67mol of aluminum aqueous solution within 60min, neutralize with 30% sulfuric acid aqueous solution to obtain solid precipitation, cool, filter, wash with water, and dry; obtain 1253g of aluminum diethylphosphinate, yield 96.4%; bulk tap density It is 610g / L; the product particle size (μm) distribution is: D(10): 34; D(50): 71; D(90): 128;

[0044] IR: 779CM -1 ,...

Embodiment 2

[0046] Same as in Example 1, potassium hydroxide was used as the basic compound, 4200 g and 30 mol of a 40% KOH aqueous solution were added to the reactor to obtain 1246 g of aluminum diethylphosphinate, with a yield of 95.8%; the bulk tap density was 640 g / L; Product particle size (μm) distribution: D(10): 39; D(50): 77; D(90): 122.

Embodiment 3

[0048]Same as in Example 1, aluminum chloride is used for the metal compound, hydrochloric acid is used for the acid solution, 2010 g of an aqueous solution with a mass fraction of 40% aluminum chloride hexahydrate is made, and 3.33 mol is added within 60 minutes, and neutralized with 17% hydrochloric acid to obtain diethyl Aluminum phosphinate 1248g, yield 96.0%; bulk tap density 600g / L; product particle size (μm) distribution: D(10): 38; D(50): 77; D(90): 121.

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Abstract

The invention discloses a preparation method and application of dialkyl phosphinate with high density and large diameter. The method comprises steps of: a) adding an alkali compound aqueous solution into a dialkyl phosphinic acid and / or dialkyl phosphinic acid alkali metal salt aqueous solution, and adjusting the solution to an alkaline state to obtain a dialkyl phosphinate aqueous solution under alkaline conditions; b) reacting the metal compound aqueous solution with the dialkyl phosphinate aqueous solution under alkaline conditions; and c) neutralizing the solution with acid to obtain the dialkyl phosphinate shown such as a formula (I). R1, R2 are the same or different, and represent methyl, ethyl, butyl, pentyl, cyclopentyl, cyclohexyl or octyl; M represents Mg, Ca, Al, Fe, Zn, Sb, Sn, Ge, Ti, Zr or Sr; and m is 2-4. The prepared dialkyl phosphinate has large diameter and high bulk density; the method has simple process, convenient operation and easy product packaging, and can greatly reduce dust pollution during the production process; and the product can be used as an environment-friendly, efficient, halogen-free flame retardant in polymer materials.

Description

technical field [0001] The invention relates to the field of flame retardant synthesis, in particular to a preparation method and application of a high-density, large-particle-diameter dialkylphosphinate. Background technique [0002] Dialkylphosphinic acid and dialkylphosphinate are high-efficiency halogen-free flame retardants with low bulk density, small amount of flame retardant, good mechanical properties, good color, low smoke density, CTI( Compared with the tracking index), the value can be as high as 600V, and it is widely used in thermoplastic and thermosetting plastics such as polyamide, polyester, unsaturated resin, epoxy resin, polyurethane, etc. [0003] Hoechst AG of Germany applied for a patent DE4430932 in 1994, disclosing the preparation of dialkylphosphinic aluminum and dialkylphosphine calcium phosphate with dialkylphosphinic acid and aluminum hydroxide or calcium hydroxide. And disclosed their application as flame retardants in polyester molding composit...

Claims

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Application Information

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IPC IPC(8): C07F9/30C08K5/5313C08K7/14C08L67/02
Inventor 陈林柴生勇李积德孔蕾卢昌利
Owner ZHUHAI WANTONG CHEM
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