Preparation method of 3,3-bi(nitrine methyl) epoxybutane and tetrahydrofuran copolymer
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A technology of butylene oxide and tetrahydrofuran, applied in 3 fields, achieves the effect of complete azidation reaction, simple method, and accelerated reaction process
Inactive Publication Date: 2015-05-27
天元航材(营口)科技股份有限公司
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example 1
[0016] Take a 500ml four-neck flask, equipped with mechanical stirring, constant pressure dropping funnel, low-temperature water bath, and thermometer, add 26g of dichloromethane, add 1.5g of 1,4-butanediol, 3.08g of boron trifluoride etherate complex, 13.6 g tetrahydrofuran, prepare the initiator at room temperature, lower the temperature to 0°C, add 24g of 3,3-bis(chloromethyl)butylene oxide dropwise within 1 to 2 hours, react at a temperature of 0±2°C for 12 hours, and then 50 g of dichloromethane was added for extraction, and 200 g of water was added for washing to obtain a copolymer of 3,3-bis(azidomethyl)butylene oxide and tetrahydrofuran.
[0017] Weigh 0.5g of sodium iodide, add 3,3-bis(azidomethyl)butylene oxide and tetrahydrofuran copolymer solution, add 20g of sodium azide at room temperature, react for 10 hours, add 200g of water After washing with water for 0.5 hour, the solvent was distilled off to obtain a copolymer of 3,3-bis(azidomethyl)butylene oxide and tetr...
example 2
[0019] Take: 1000ml four-necked flask equipped with mechanical stirring, constant pressure dropping funnel, low-temperature water bath, thermometer, add 52g of dichloroethane, add 2.6g of 1,4-butanediol, 6.1g of boron trifluoride etherate complex , 27.2g tetrahydrofuran, prepare the initiator at room temperature, cool down to -2°C, add 48g of 3,3-bis(chloromethyl)butylene oxide dropwise within 1 to 2 hours, and react at a temperature of 0±2°C for 18 hour, then through extraction and neutralization, 3,3-bis(chloromethyl)epoxybutylene tetrahydrofuran copolymer was obtained;
[0020] Weigh 1.5g of sodium iodide, add 3,3-bis(chloromethyl)butylene oxide tetrahydrofuran copolymer solution, add 40g of sodium azide at room temperature, react for 12 hours, add 200g of water and wash with water for 0.5 hours, the solvent was distilled off to obtain 3,3-bis(azidomethyl)epoxybutylene tetrahydrofuran copolymer.
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Abstract
The invention discloses a preparation method of a 3,3-bi(nitrine methyl) epoxybutane and tetrahydrofuran copolymer, relates to a preparation method of the 3,3-bi(nitrine methyl) epoxybutane and tetrahydrofuran copolymer, and in particular relates to a method for preparing the 3,3-bi(nitrine methyl) epoxybutane and tetrahydrofuran copolymer by performing ring opening copolymerization and catalytic nitrogenization on 3,3-bi(chloromethyl) epoxybutane. The method is simple and easy to carry out. Because a method for preparing bi(chloromethyl) polyether at first and nitriding at last to obtain a nitrine rubber product is adopted, a high-sensitivity nitrine monomer purification step is avoided, the safety hidden troubles of operation site are eliminated, and the problem of an existing production method is solved. In a process for preparing the nitrine rubber by nitrogenization of the bi(chloromethyl) polyether, a method of addition of sodium iodide is adopted, and double-decomposition exchange reaction on iodine atoms of halogen elements and chloride atoms in the bi(chloromethyl) polyether is utilized, so that a nitrogenization reaction process is accelerated, and the complete nitrogenization reaction is carried out; and therefore, the reaction effect is achieved and the product quality is greatly improved.
Description
technical field [0001] The present invention relates to a kind of preparation method of 3,3-bis(azidomethyl)butylene oxide and tetrahydrofuran copolymer, specifically is cyclized product monomer 3,3-bis(chloromethyl)butylene oxide , A method for preparing 3,3-bis(azidomethyl)butylene oxide and tetrahydrofuran copolymer through ring-opening copolymerization and catalytic azidation reaction. Background technique: [0002] Since the discovery of azido acid in the nineteenth century, azides have aroused great interest in the chemical community, and people have done extensive research on the synthesis methods, structure determination and applications of azides. Azide polyether can endow the propellant with excellent energy performance and good mechanical properties, and can reduce the detectable signal of the propellant, and the sensitivity of PBT azide propellant is low. The use of this azide glue is the development of a new generation of high-energy, insensitivity and low One ...
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