CN104650433A - Preparation method of composite flame retardant used in flame-retarding polyolefin - Google Patents

Preparation method of composite flame retardant used in flame-retarding polyolefin Download PDF

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Publication number
CN104650433A
CN104650433A CN201310588575.5A CN201310588575A CN104650433A CN 104650433 A CN104650433 A CN 104650433A CN 201310588575 A CN201310588575 A CN 201310588575A CN 104650433 A CN104650433 A CN 104650433A
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CN
China
Prior art keywords
zinc
aqueous solution
ethanediamine
flame retardant
composite flame
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201310588575.5A
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Chinese (zh)
Inventor
古朝雄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
QINGDAO NPA INDUSTRY Co Ltd
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QINGDAO NPA INDUSTRY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by QINGDAO NPA INDUSTRY Co Ltd filed Critical QINGDAO NPA INDUSTRY Co Ltd
Priority to CN201310588575.5A priority Critical patent/CN104650433A/en
Publication of CN104650433A publication Critical patent/CN104650433A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/17—Amines; Quaternary ammonium compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/16—Nitrogen-containing compounds
    • C08K5/34—Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477—Six-membered rings
    • C08K5/3492—Triazines
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/387—Borates

Abstract

The invention discloses a preparation method of a composite flame retardant used in flame-retarding polyolefin. The preparation method includes following processes: (1) adding zinc vitriol to a phosphoric acid aqueous solution to prepare a zinc phosphate aqueous solution; (2) adding ethanediamine to water to prepare an ethanediamine aqueous solution; (3) adding the ethanediamine aqueous solution to the zinc phosphate aqueous solution with stirring and mixing uniformly at 25 DEG C; (4) carrying out a reaction for 2 h and allowing the reaction system to stand to separate out an ethanediamine zinc diphosphate crystal; (5) performing suction filtration and washing a product, and drying the product to obtain ethanediamine zinc diphosphate-I; and (6) finally mixing melamine pyrophosphate, the ethanediamine zinc diphosphate-I and low-water aluminum borate in a high-speed mixing machine with surface treatment by a coupling agent to obtain a halogen-free composite flame retardant. In the composite flame retardant, the low-water aluminum borate is combined with the melamine pyrophosphate and the ethanediamine zinc diphosphate-I to enhance a flame-retarding and smoke-inhibiting performance. The composite flame retardant can promote charcoal forming and stabilize a charcoal layer, can delay an ignition time of a material, can reduce smoke generation and smoke escape speed of the material, can increase mass retaining rate of the material and can achieve a better flame-retarding and smoke-inhibiting performance in a condensed phase.

Description

For the preparation method of the composite flame-retardant agent of fire retardant polyolefin
 
Technical field
The present invention relates to a kind of preparation method of composite flame-retardant agent, be specifically related to a kind of preparation method of the composite flame-retardant agent for fire retardant polyolefin.
 
Background technology
In the fire retardant that polyolefine used in the past, halogenated flame retardant is most widely used, but the problem having the amount of being fuming more when burning, be fuming when can cause greatly fire to the serious secondary disaster of the person; With when aluminium hydroxide, magnesium hydroxide then must addition comparatively great talent have flame retardant effect, therefore have shortcomings such as reducing plastics flexible nature.
 
Summary of the invention
The object of the invention is to, provide a kind of preparation method of the composite flame-retardant agent for fire retardant polyolefin, the composite flame-retardant agent obtained, flame retarding and smoke suppressing properties improves, postpone the ignitor firing time of material, reduce the raw cigarette of material and cigarette effusion speed, improve quality of materials retention rate.
The preparation method of the described composite flame-retardant agent for fire retardant polyolefin, it comprises the following steps:
One, in phosphate aqueous solution, add zinkosite, produce phosphoric acid zinc aqueous solution;
Two, in water, add quadrol, be mixed with ethylenediamine solution, add in above-mentioned phosphoric acid zinc aqueous solution, 25 DEG C are uniformly mixed, and reaction 2h, leaves standstill, and separate out quadrol bisphosphate zinc crystal, suction filtration, washing, is drying to obtain quadrol bisphosphate zinc-I;
Three, melamine pyrophosphate, quadrol bisphosphate zinc-I and low water aluminum borate high-speed mixer mix, and use coupling agent surface treatment simultaneously, obtain Halogenless composite fire retardant.
The preparation method of the composite flame-retardant agent for fire retardant polyolefin provided by the invention, its beneficial effect is, this composite flame-retardant agent has coordinated low water aluminum borate in melamine pyrophosphate and quadrol bisphosphate zinc-I, enhances flame retarding and smoke suppressing properties, promote into charcoal, stablize layer of charcoal, postpone the ignitor firing time of material, reduce the raw cigarette of material and cigarette effusion speed, improve quality of materials retention rate, prevent molten drop, suppress to glow, play better flame-retardant smoke inhibition effect at condensed phase.
 
Embodiment
Below in conjunction with an embodiment, the preparation method of the composite flame-retardant agent for fire retardant polyolefin provided by the invention is described in detail.
 
Embodiment
One, in the phosphate aqueous solution of dilution, under agitation add zinkosite, produce phosphoric acid zinc aqueous solution;
Two, in water, quadrol is added, be mixed with ethylenediamine solution, add in above-mentioned phosphoric acid zinc aqueous solution, 25 DEG C are uniformly mixed, reaction 2h, stop stirring, leave standstill, separate out quadrol bisphosphate zinc crystal, suction filtration, filter cake washes with water, and filter cake is dry 3h in the electric drying oven with forced convection of 125 DEG C, obtains quadrol bisphosphate zinc-I;
Three, melamine pyrophosphate, quadrol bisphosphate zinc-I and low water aluminum borate high-speed mixer are mixed, use coupling agent surface treatment simultaneously, obtain Halogenless composite fire retardant.

Claims (1)

1. for a preparation method for the composite flame-retardant agent of fire retardant polyolefin, it is characterized in that: it comprises the following steps:
One, in phosphate aqueous solution, add zinkosite, produce phosphoric acid zinc aqueous solution;
Two, in water, add quadrol, be mixed with ethylenediamine solution, add in above-mentioned phosphoric acid zinc aqueous solution, 25 DEG C are uniformly mixed, and reaction 2h, leaves standstill, and separate out quadrol bisphosphate zinc crystal, suction filtration, washing, is drying to obtain quadrol bisphosphate zinc-I;
Three, melamine pyrophosphate, quadrol bisphosphate zinc-I and low water aluminum borate high-speed mixer mix, and use coupling agent surface treatment simultaneously, obtain Halogenless composite fire retardant.
CN201310588575.5A 2013-11-21 2013-11-21 Preparation method of composite flame retardant used in flame-retarding polyolefin Pending CN104650433A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310588575.5A CN104650433A (en) 2013-11-21 2013-11-21 Preparation method of composite flame retardant used in flame-retarding polyolefin

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310588575.5A CN104650433A (en) 2013-11-21 2013-11-21 Preparation method of composite flame retardant used in flame-retarding polyolefin

Publications (1)

Publication Number Publication Date
CN104650433A true CN104650433A (en) 2015-05-27

Family

ID=53242099

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310588575.5A Pending CN104650433A (en) 2013-11-21 2013-11-21 Preparation method of composite flame retardant used in flame-retarding polyolefin

Country Status (1)

Country Link
CN (1) CN104650433A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105199185A (en) * 2015-10-28 2015-12-30 辽宁石油化工大学 Environment-friendly polyolefin flame retardant
CN114250055A (en) * 2021-12-16 2022-03-29 山东北方现代化学工业有限公司 Single-component halogen-free flame-retardant silane modified polyurethane sealant and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105199185A (en) * 2015-10-28 2015-12-30 辽宁石油化工大学 Environment-friendly polyolefin flame retardant
CN114250055A (en) * 2021-12-16 2022-03-29 山东北方现代化学工业有限公司 Single-component halogen-free flame-retardant silane modified polyurethane sealant and preparation method thereof
CN114250055B (en) * 2021-12-16 2024-02-27 山东北方现代化学工业有限公司 Single-component halogen-free flame-retardant silane modified polyurethane sealant and preparation method thereof

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Application publication date: 20150527