Additive composition for polymer, preparation method of additive composition and flame-retardant thermoplastic polymer molding material by using additive composition

A polymer and additive technology, which is applied in the field of flame-retardant thermoplastic polymer molding materials, can solve the problems of screw corrosion in compounding combination devices, reduce energy and labor losses, have practicality, and reduce equipment processing costs.

Inactive Publication Date: 2015-02-25
ZHUHAI WANTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the problem of the whiteness of the flame retardant polymer added with dialkyl phosphinate and the corrosion of the molding composition to the screw of the compounding assembly during processing, th

Method used

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  • Additive composition for polymer, preparation method of additive composition and flame-retardant thermoplastic polymer molding material by using additive composition
  • Additive composition for polymer, preparation method of additive composition and flame-retardant thermoplastic polymer molding material by using additive composition
  • Additive composition for polymer, preparation method of additive composition and flame-retardant thermoplastic polymer molding material by using additive composition

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Embodiment 1: the preparation of one-component A aluminum diethylphosphinate

[0063] Hydroboration of 1060.0g (10mol) sodium hypophosphite monohydrate, 9.1g (0.3%mol hypophosphite ion) 1,1-di-tert-butylperoxy-3,3,5-trimethylcyclohexane, 3.0g Add sodium and 1500g water into the autoclave, evacuate it, replace it with nitrogen for 3 times, evacuate it, then fill it with ethylene through a pressure reducer and control the pressure at 2.0MPa, heat to 95°C for 5h, then raise the temperature to 100°C, and continue for 5h Add 18.1g (0.6% mol hypophosphite ion) of 1,1-di-tert-butylperoxy-3,3,5-trimethylcyclohexane, heat up to 100°C, keep warm for 1h, cool and vent to obtain diethyl The aqueous solution of sodium phosphinate is 3169.3g, which is equivalent to 579.1g of ethylene absorption (103.4% of the theoretical amount).

[0064] 31 P-NMR analysis:

[0065] Diethylphosphinic acid mol content: 98.1%

[0066] Ethylphosphonous acid mol content: 0%

...

Embodiment 2

[0070] Embodiment 2: the preparation of one-component B aluminum ethyl phosphinate

[0071] 1171.4g (10mol) 70% phosphorous acid, 9.1g (0.3%mol phosphorous acid) 1,1-di-tert-butylperoxy-3,3,5-trimethylcyclohexane and 3.0g sodium borohydride, Evacuate, replace with nitrogen for 5 times, evacuate, then fill with ethylene through the pressure reducer and control the pressure to 2.0MPa, heat to 90°C for 10h, and continuously add 18.1g (0.6% mol phosphorous acid) 1,1- Di-tert-butyl peroxide-3,3,5-trimethylcyclohexane, heated up to 100°C, kept warm for 1 hour, cooled and vented to obtain 1487.5g of ethylphosphonous acid solution, equivalent to ethylene absorption of 285.9g ( 102.1% of the theoretical amount).

[0072] 31 P-NMR analysis:

[0073] Ethylphosphonous acid mol content: 98.8%

[0074] Phosphorous acid mol content: 0%

[0075] Other mol content: 1.2%

[0076] Take 223.1g of its solution, add 1000g of water, heat and stir to 90°C, add dropwise 20% octadecahydrate alu...

Embodiment 3

[0077] Embodiment 3: the preparation of one-component C aluminum phosphite

[0078] Drop 1110.0g, 20wt% (0.33mol) aluminum sulfate aqueous solution into 1080g, 20wt% (1.0mol) sodium phosphite pentahydrate aqueous solution at a constant temperature of 80°C within 1 hour, filter, and wash the obtained filter cake three times with 1000ml water to obtain Aluminum phosphite 94.27g, yield: 95.22%.

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Abstract

The invention discloses an additive composition for a polymer, a preparation method of the additive composition and a flame-retardant thermoplastic polymer molding material by using the additive composition. The additive composition is prepared from the following components in percentage by weight: 80-99.99 percent of a component A which is dialkyl hypophosphite with a structure as shown in a formula (I), 0-20 percent of a component B which is alkyl phosphite with a structure as shown in a formula (II), and 0-0.9 percent of a component C which is phosphite with a structure as shown in a formula (III), wherein the component B and the component C are not 0 percent by weight at the same time, and the total amount of the components A, B and C is 100 percent by weight all the time. The additive is applied to a polymer, so that the corrosion degree of a flame-retardant polymer on screws of a mixing combination device can be greatly reduced, equipment processing cost can be reduced, energy and labor loss caused by frequently changing screws in the processing process can be reduced, and the whiteness of a polymer component obtained through extrusion molding is superior to that of a conventional dialkyl hypophosphite modified polymer component.

Description

technical field [0001] The present invention relates to an additive composition for polymers, in particular to a dialkylphosphinate containing alkylphosphinate and / or phosphite, a process for its preparation and a flame retardant composition thereof Thermoplastic polymer molding material. Background technique [0002] Dialkylphosphinates, widely used as flame retardants, are known to be synthesized by different methods. For example, patent DE4430932 discloses that disubstituted phosphinic acid metal salt is used as a flame retardant in polyester, and two patents, DE19910232 and US6248921, disclose a preparation method of disubstituted phosphinic acid metal salt. U.S. Patent US6359171B1 discloses a method for preparing aluminum dialkylphosphinate. In this method, yellow phosphorus is first used to synthesize monoalkylphosphinate, and then vinylation is initiated by free radicals, followed by hydrolysis to obtain acid, and then reacted with aluminum salt to obtain Aluminum d...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C08K5/5393C08K3/32C08L67/02C08K7/14
CPCC08K3/32C08K5/5313C08K5/5317C08K2003/329C08K5/5393
Inventor 李积德柴生勇卢昌利陈林孔蕾李岩
Owner ZHUHAI WANTONG CHEM
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