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Circulating micro-reaction device and method for producing brominated polystyrene

A technology of brominated polystyrene and micro-reaction devices, applied in chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical fixed reactors, etc., can solve the problem of rapid and uniform mixing of reactants Difficult to realize, limited mass transfer and heat transfer capacity, low production efficiency and other problems, to achieve high production efficiency, increase thermal weight loss temperature, and process safety effects

Inactive Publication Date: 2020-04-21
山东旭锐新材股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can prepare brominated polystyrene products with high selectivity, the production efficiency is seriously low and the safety risk is high. Therefore, continuous and efficient production equipment is very important for the production of brominated polystyrene products
From the perspective of chemical reaction principle, the electrophilic substitution reaction process of polystyrene benzene ring itself is a fast reaction process, so the formation of by-products is mainly due to the fact that the rapid and uniform mixing of reactants is not easy to achieve, which is limited by the mass and heat transfer capabilities of traditional chemical equipment. Can only use conservative slow drop production

Method used

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  • Circulating micro-reaction device and method for producing brominated polystyrene
  • Circulating micro-reaction device and method for producing brominated polystyrene
  • Circulating micro-reaction device and method for producing brominated polystyrene

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Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1 A kind of circulating micro-reaction method of producing brominated polystyrene

[0035] (1) Preparation of brominating agent solution D

[0036] Prepare 2000kg of bromine / bromochloromethane solution with a mass fraction of 20% as brominating agent solution D.

[0037] (2) Add polystyrene and catalyst

[0038] Add 2000kg mass fraction of 5% polystyrene solution and 1kg AlCl in 5000L circulating reactor 1 3 powder, stir and mix well to obtain polymer solution C, and lower the temperature of polymer solution C to -10°C;

[0039] Described polystyrene, molecular weight is 2000g / mol;

[0040] Described polystyrene solution, solvent is bromochloromethane;

[0041] Turn on the circulation pump 2, the front heat exchanger 3 and the rear heat exchanger 5, and firstly enter the polymer solution C from the bottom of the circulation reactor 1 through the front heat exchanger 3, the micro mixer 4, and the rear heat exchanger 5. The reactor 1 is circulated for circ...

Embodiment 2

[0047] Embodiment 2 A kind of circulation micro-reaction method of producing brominated polystyrene

[0048] (1) Preparation of brominating agent solution D

[0049] Preparation 2667kg mass fraction is 30% bromine / chloroform solution as brominating agent solution D;

[0050] (2) Add polystyrene and catalyst

[0051] In the 5000L circulating reactor 1, add 2000kg mass fraction to be 10% polystyrene solution and catalyst (8kgAlCl 3 powder and 8kgSnCl 4 powder mixture), after stirring and mixing, the polymer solution C was obtained, and the temperature of the polymer solution C was lowered to -2°C.

[0052] The polystyrene has a molecular weight of 100000g / mol;

[0053] For the polystyrene solution, the solvent is chloroform.

[0054] Turn on the circulation pump 2, the front heat exchanger 3 and the rear heat exchanger 5, and firstly enter the polymer solution C from the bottom of the circulation reactor 1 through the front heat exchanger 3, the micro mixer 4, and the rear ...

Embodiment 3

[0060] Embodiment 3 A kind of circulating micro-reaction method of producing brominated polystyrene

[0061] (1) Preparation of brominating agent solution D

[0062] Prepare 750kg bromine / mixed solvent (1:1 mass ratio of bromochloromethane and dichloromethane) solution with a mass fraction of 80% as brominating agent solution D.

[0063] (2) Add polystyrene and catalyst

[0064] In the 5000L circulating reactor 1, add 2000kg mass fraction to be 10% polystyrene solution and catalyst (7.5kgAlCl 3 powder and 7.5kg metal Sn powder), after stirring and mixing, the polymer solution C was obtained, and the temperature of the polymer solution C was lowered to -8°C.

[0065] Described polystyrene, molecular weight is 200000g / mol;

[0066] The solvent of the polystyrene solution is a mixed solvent, which is mixed with bromochloromethane and dichloromethane according to a mass ratio of 1:1.

[0067] Turn on the circulation pump 2, the front heat exchanger 3 and the rear heat exchange...

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Abstract

The invention discloses a circulating micro-reaction device for producing brominated polystyrene. The device is formed by end-to-end tandem connection of a circulating reaction kettle, a circulating pump, a front heat exchanger, a micro-mixer and a rear heat exchanger. The invention also discloses a circulating micro-reaction method for producing brominated polystyrene. A low-temperature bromination reaction of polystyrene is carried out in the micro-reaction device; a polymer solution circularly flows between the circulating reaction kettle and the micro-mixer; the micro-mixer plays a role inenhancing mixing between a brominating agent and the polystyrene solution; and the front heat exchanger and the rear heat exchanger are used for strictly controlling the reaction temperature, so thetemperature uniformity of a reaction system and the selectivity of bromine substitution sites are guaranteed. The bromine content of brominated polystyrene produced by the micro-reaction device is greater than or equal to 66%, the 1% thermal weight loss temperature is greater than or equal to 348 DEG C, and the 5% thermal weight loss is greater than or equal to 372 DEG C.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a circulating micro-reaction device for producing brominated polystyrene. Background technique [0002] Brominated polystyrene is an additive polymer brominated flame retardant, which has the advantages of high bromine content, low toxicity, excellent heat resistance and impact resistance, good fluidity, and no frosting. It is widely used in nylon, Flame retardant processing of high temperature resistant resins such as polyester. [0003] Brominated polystyrene is mainly completed by the electrophilic substitution reaction of polystyrene and brominating agent. Taking bromine as the bromination agent as an example, the raw material bromine first dissociates into Br under the action of a Lewis acid catalyst. + ions, and then the hydrogen on the benzene ring is replaced to complete the bromination, and the reaction equation is shown in formula 1. [0004] [0...

Claims

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Application Information

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IPC IPC(8): B01J19/18B01J19/00C08F8/22C08F8/20C08F112/08
CPCB01J19/0013B01J19/0093B01J19/18C08F8/20C08F8/22C08F112/08
Inventor 王凯骆广生王德强杨凯王强李金忠杨振振
Owner 山东旭锐新材股份有限公司