CN102250382B - Preparation method of high thermostable eight bromo ether - Google Patents
Preparation method of high thermostable eight bromo ether Download PDFInfo
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- CN102250382B CN102250382B CN2011101266691A CN201110126669A CN102250382B CN 102250382 B CN102250382 B CN 102250382B CN 2011101266691 A CN2011101266691 A CN 2011101266691A CN 201110126669 A CN201110126669 A CN 201110126669A CN 102250382 B CN102250382 B CN 102250382B
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Abstract
Belonging to the technical field of preparing high thermostable materials by adding specific thermostable components into ordinary eight bromo ether, the invention relates to a preparation method of high thermostable eight bromo ether. The method of the invention employs a composite thermostable auxiliary agent of zine stearate/barium stearate or zine stearate/calcium stearate in a specific amount and a specific proportion, a composite anti-oxidant in a specific amount and a specific proportion, adds a specific kind of coupling agent, and adopts a high-speed mixer for high-speed stirring and blending so as to prepare a high thermostable eight bromo ether material, the 1% weight loss temperature of which is increased by 20-30DEG C.
Description
Technical field
The present invention relates to a kind of preparation method of high heat stability eight bromo ether, belong to common eight bromo ether through adding the technical field of specific stabilizing component acquisition high thermal stability material.
Background technology
The full name of eight bromo ether is tetrabromo-bisphenol-two (2, the 3-dibromopropyl) ether, is a kind of bromide fire retardant commonly used, in materials such as Vestolen PP 7052, PS, add and with the composite use of antimony compounds, can make material obtain excellent flame-retardant.Because eight bromo ether has the bromine content more than 67%, and fusing point has good consistency more than 105 ℃ with polyolefine material.
But as the flame retardant material; The eight bromo ether molecule contains eight bromine atoms on aliphatic chain, this material is in the course of processing, and this bromine atoms is easy to eliminate reaction with the Wasserstoffatoms generation hydrogen bromide that is close on the fatty carbon; After hydrogen bromide produces with the fracture of other bromine carbon bonds on the further catalysis eight bromo ether molecule; Cause the eight bromo ether thermostability to reduce, make material easy thermal destruction variable color excessively in the course of processing of adding eight bromo ether, hinder this material and using in the field widely.
For thermostability and the decomposition temperature that improves eight bromo ether, related to the related process method in the patent of Lianyun Harbour seawater chemical industry application in 2006, its patent name is the method that environmental friendliness prepares high thermal decomposition temperature octobromo ether, patent No. CN100398503C.The method that this patent improves the eight bromo ether thermostability is in the process of preparation eight bromo ether, to have added ionic emulsifying agent, nonionic emulsifier or amphoterics; And added and helped thermo-stabilizer; Comprise Sionit, tricarbimide glycidyl ester, 1, two (beta-amino butenoic acid) esters of 4-butyleneglycol.
2009, HeFei University of Technology's journal the 32nd volume the 6th phase 837-840 page or leaf reported that a kind of method that adopts microcapsule to coat improves the method for eight bromo ether thermostability.This method makes the aminoresin prepolymer through trimeric cyanamide and formolite reaction and coats the eight bromo ether particle, and its temperature of initial decomposition of the eight bromo ether after the coating is brought up to more than 240 ℃ from 160 ℃.
Aforesaid method is for improving eight bromo ether thermostability aspect complex process, and is high to the eight bromo ether processing cost.
Summary of the invention
For obtain a kind of simply, eight bromo ether thermostabilization method efficiently; The present invention adopts the stearate compounds; Through absorb the micro-hydrogen bromide that eight bromo ether discharges in the heated and degraded process; Prevent the catalyzed degradation effect of hydrogen bromide, thereby play the stable effect of eight bromo ether molecule to the eight bromo ether molecule; And, avoid the existence of oxyradical to bring out the fracture of bromine carbon bond through adding antioxidant systems, delay the eight bromo ether degraded and generate hydrogen bromide.
The process that the present invention prepares the eight bromo ether of thermostabilization is with weighings according to a certain percentage such as eight bromo ether, heat stabilizer system, antioxidant systems, coupling agents; Add then impeller at a certain temperature the high speed solid phase mix, obtain a kind of eight bromo ether product of thermostabilization.
Used synthesis material: tetrabromo-bisphenol-two (2, the 3-dibromopropyl) ethers (purity＞96%, technical grade), Zinic stearas (purity＞98%; Technical grade), calcium stearate (purity＞98%, technical grade), barium stearate (purity＞98%, technical grade); Coupling agent 3-aminopropyl triethoxysilane (being called for short KH550) (purity＞98%, technical grade), 3-methacryloxypropyl trimethoxy silane (being called for short KH570) (purity＞98%, technical grade); Oxidation inhibitor four-[β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid]-pentaerythritol ester (is called for short antioxidant 1010, purity＞98%; Technical grade), tricresyl phosphite-(2; The 4-di-tert-butyl-phenyl) ester (being called for short oxidation inhibitor 168, purity＞98%, technical grade).
Concrete preparation method:
The configuration of compound thermally-stabilised auxiliary agent: a kind of and Zinic stearas in selection barium stearate or the calcium stearate is in the composite (Zinic stearas/barium stearate of 1: 2～2: 1 ratio of mass ratio; Zinic stearas/calcium stearate); Wherein reasonable ratio is 1: 1, stirs.
The configuration of composite antioxidant: according to mass ratio configuration in 1: 4～4: 1 antioxidant systems, wherein reasonable ratio is 1: 2, mixes with antioxidant 1010 and 168.
The preparation of high thermal stability eight bromo ether: take by weighing 100 parts of eight bromo ethers; Add 1～5 part of the compound thermally-stabilised auxiliary agent configure, add composite antioxidant 0.5-5 part, add a kind of among 0.5～4 part of coupling agent KH550 or the KH570; It is even to add the impeller high-speed stirring; Test eight bromo ether temperature of initial decomposition, the temperature of initial decomposition of former eight bromo ether is 250～260 ℃, the eight bromo ether temperature of initial decomposition of high heat stability system (material 1% thermal weight loss) rises 20～30 ℃; Reach 270～290 ℃, obtained to have the eight bromo ether material of high heat stability performance.
Characteristics such as the present invention adopts the method for simple blend to prepare the eight bromo ether auxiliary agent of high heat stability, has avoided the front document to prepare the complicated technology and the method for high heat stability eight bromo ether, simplifies preparation flow and has the preparation efficiency height, and is simple to operate; Adopt composite antioxidant and compound thermally-stabilised auxiliary agent coupling, at first avoided thermal oxidation to cause the fracture of bromine carbon bond, and the sorption of hydrogen bromide has been avoided the accelerate decompsn of eight bromo ether through compound thermally-stabilised auxiliary agent; Prepared eight bromo ether temperature of initial decomposition improves significantly, and thermal stability and auxiliary agent proportional curve are seen accompanying drawing 1 and accompanying drawing 2.
Figure of description
Compound thermally-stabilised promoter addition of accompanying drawing 1 Zinic stearas/calcium stearate and eight bromo ether temperature of initial decomposition relation curve added 2: 1 oxidation inhibitor of 2 parts of mass ratioes 168: 1010, added 1 part of coupling agent KH570
Compound thermally-stabilised promoter addition of accompanying drawing 2 Zinic stearass/barium stearate and eight bromo ether temperature of initial decomposition relation curve added 2: 1 oxidation inhibitor of 2 parts of mass ratioes 168: 1010, added 1 part of coupling agent KH570
Embodiment:
Embodiment 1 takes by weighing 100 parts of eight bromo ethers; Zinic stearas and barium stearate are disposed 3 part according to mass ratio at 1: 1; Oxidation inhibitor 168 and antioxidant 1010 are according to 2 parts of 2: 1 proportional arrangement; Add 1 part of coupling agent KH570, put into impeller and stir, 1% weightless temperature of initial decomposition of test material is 285 ℃.
Embodiment 5 takes by weighing 100 parts of eight bromo ethers; Zinic stearas and calcium stearate are disposed 4 part according to mass ratio at 1: 1; Oxidation inhibitor 168 and antioxidant 1010 are according to 2 parts of 1: 1 proportional arrangement; Add 1 part of coupling agent KH570, put into impeller and stir, 1% weightless temperature of initial decomposition of test material is 285 ℃.
Embodiment 6 takes by weighing 100 parts of eight bromo ethers; Zinic stearas and calcium stearate are disposed 2 part according to mass ratio at 1: 1; Oxidation inhibitor 168 and antioxidant 1010 are according to 1 part of 1: 1 proportional arrangement; Add 1 part of coupling agent KH570, put into impeller and stir, 1% weightless temperature of initial decomposition of test material is 279 ℃.
Claims (1)
1. the preparation method of a high thermal stability eight bromo ether is characterized in that through in eight bromo ether, adding compound thermally-stabilised auxiliary agent, composite antioxidant and coupling agent component by a certain percentage and the method through the impeller blend prepares; Wherein employed compound thermally-stabilised auxiliary agent is Zinic stearas/barium stearate system or 1: 2～2: 1 Zinic stearas/calcium stearate system of mass ratio of mass ratio 1: 2～2: 1; Antioxidant 1010 and oxidation inhibitor 168 are according to mass ratio configuration in 1: 4～4: 1 in the employed composite antioxidant; Described certain proportion is for adding 1～5 part of compound thermally-stabilised auxiliary agent, adding a kind of among 0.5-5 part composite antioxidant and 0.5～4 part of coupling agent KH550 or the KH570 in 100 parts eight bromo ether.
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| CN2011101266691A CN102250382B (en) | 2011-05-17 | 2011-05-17 | Preparation method of high thermostable eight bromo ether |
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| CN2011101266691A CN102250382B (en) | 2011-05-17 | 2011-05-17 | Preparation method of high thermostable eight bromo ether |
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| CN102250382A CN102250382A (en) | 2011-11-23 |
| CN102250382B true CN102250382B (en) | 2012-10-31 |
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| CN108102213B (en) * | 2017-11-10 | 2021-01-26 | 金发科技股份有限公司 | Flame-retardant polypropylene composition and preparation method and application thereof |
| CN114773671B (en) * | 2022-04-25 | 2023-10-20 | 北京工商大学 | Spray drying preparation method of methyl octabromoether microcapsule and flame-retardant XPS material thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633843A (en) * | 2009-07-04 | 2010-01-27 | 山东兄弟科技股份有限公司 | Preparation method of bromine nitrogen series composite flame retardant |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633843A (en) * | 2009-07-04 | 2010-01-27 | 山东兄弟科技股份有限公司 | Preparation method of bromine nitrogen series composite flame retardant |
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Granted publication date: 20121031 Termination date: 20140517 |