Additive composition for polymer as well as preparation method for additive composition for polymer and flame retardant thermoplastic polymer molding material constituted by additive composition for polymer

A thermoplastic polymer and additive technology, applied in the field of flame retardant thermoplastic polymer molding materials, can solve problems such as screw corrosion of compounding devices

Active Publication Date: 2015-04-08
肖群
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] 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, the object...

Method used

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  • Additive composition for polymer as well as preparation method for additive composition for polymer and flame retardant thermoplastic polymer molding material constituted by additive composition for polymer
  • Additive composition for polymer as well as preparation method for additive composition for polymer and flame retardant thermoplastic polymer molding material constituted by additive composition for polymer
  • Additive composition for polymer as well as preparation method for additive composition for polymer and flame retardant thermoplastic polymer molding material constituted by additive composition for polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0075] Embodiment 1: the preparation of one-component A aluminum diethylphosphinate

[0076] Hydroboration of 636.0g (6mol) sodium hypophosphite monohydrate, 5.5g (0.3%mol hypophosphite ion) 1,1-di-tert-butylperoxy-3,3,5-trimethylcyclohexane, 1.8g Add sodium and 900g 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 to 2.0MPa, heat to 95°C for 5h, then raise the temperature to 100°C, and continue for 5h Add 10.9g (0.6% mol hypophosphite ion) 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 was 1902.7g, equivalent to 348.5g of ethylene absorption (103.7% of the theoretical amount).

[0077] 31 P-NMR analysis:

[0078] Diethylphosphinic acid mol content: 98.3%

[0079] Ethylphosphonous acid mol content: 0%

[0080] ...

Embodiment 2

[0083] Embodiment 2: the preparation of one-component C ethyl phosphonite aluminum

[0084] 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 1490.8g of ethylphosphonous acid solution, equivalent to ethylene absorption of 289.2g ( 103.3% of the theoretical amount).

[0085] 31 P-NMR analysis:

[0086] Ethylphosphonous acid mol content: 98.2%

[0087] Phosphorous acid mol content: 0%

[0088] Other mol content: 1.8%

[0089] Take 223.6g of its solution, add 1000g of water, heat and stir to 90°C, add dropwise a...

Embodiment 3

[0090] Embodiment 3: the preparation of one-component D aluminum phosphite

[0091] 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 90.8g, yield: 92.7%.

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Abstract

The invention discloses an additive composition for polymer as well as a preparation method for the additive composition for the polymer and a flame retardant thermoplastic polymer molding material constituted by the additive composition for the polymer. The additive composition for polymer comprises the following components: a component A, namely 80wt%-99.99wt% of dialkyl phosphinate with a structure as shown in a formula (I); a component B, namely 0.001wt%-0.5wt% chloride with weight content of chlorine elements in the total additive as 60-800ppm; a component C, namely 0wt%-20wt% of alkyl phosphonate with a structure as shown in a formula (II); a component D, namely 0wt%-0.9wt% of phosphite with a structure as shown in formula (III), based on 100wt% in total, wherein the weight fractions of the components C and D are not 0wt% at the same time. The additive disclosed by the invention is applied to the polymer, so that the corrosion degree of the flame retardant polymer to a mixing combined device screw is greatly lowered, the energy and labor loss caused by frequently replacing the screw in a processing process is further reduced while the equipment processing cost is lowered; the whiteness of the polymer part obtained by extrusion molding is superior to that of the polymer part modified by the normal dialkyl phosphinate.

Description

technical field [0001] The present invention relates to an additive composition for polymers, in particular to a dialkylphosphinate containing chlorine and alkylphosphinate and / or phosphite, a preparation method thereof and a composition thereof flame retardant thermoplastic polymer molding materials. 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 obtai...

Claims

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Application Information

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IPC IPC(8): C08L67/02C08K13/04C08K5/5313C08K5/5393C08K5/524C08K5/02C08K3/16C08K5/5419
CPCC08K3/16C08K3/32C08K5/5313C08K5/5393C08K7/14C08K13/02C08K13/04C08L63/00C08L67/02C08L75/04C08L77/00
Inventor 不公告发明人
Owner 肖群
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