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Method for preparing monophosphonate and biphosphonate mixed fire retardant
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A flame retardant and phosphonate technology, which is applied in the field of preparation of single and double mixed phosphonate flame retardants, can solve the problems of harsh reaction conditions, rare raw materials, and difficult control, and achieves no emission in the production process and product utilization. The effect of high rate and low viscosity
Inactive Publication Date: 2014-01-01
NANJING NORMAL UNIVERSITY +1
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Methods 2 and 3 have rare raw materials, high energy consumption, and harsh reaction conditions that are difficult to control
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Embodiment 1
[0054] Add trimethyl phosphite (P(OCH 3 ) 3 )37.2g, 1,2-dibromoethane (BrCH 2 CH 2 Br) 18.8g, catalyst I 20.25g. Turn on the condensed water, heat and stir, and start to reflux when the temperature rises to about 120°C, continue heating, the temperature gradually rises to 170°C, and the degree of reflux decreases significantly. Continue the reaction, and when there is basically no reflux, keep the temperature at 180-190°C for 1 hour. Atmospheric distillation and suction filtration gave 34.7 g of a colorless and transparent product with a total yield of 93.8%, among which the yield of tetramethyl 1,2-ethylenebisphosphonate was 55.5%.
Embodiment 2
[0056] Add trimethyl phosphite (P(OCH 3 ) 3 )37.2g, 1,2-dibromoethane (BrCH 2 CH 2 Br) 18.8g, catalyst NaI 0.25g. Turn on the condensed water, heat and stir, and start to reflux when the temperature rises to about 120°C, continue heating, the temperature gradually rises to 170°C, and the degree of reflux decreases significantly. Continue the reaction, and when there is basically no reflux, keep the temperature at 180-190°C for 1 hour. Atmospheric distillation and suction filtration gave 34.2 g of a colorless and transparent product with a total yield of 92.4%, among which the yield of tetramethyl 1,2-ethylenebisphosphonate was 63.7%.
Embodiment 3
[0058] Add trimethyl phosphite (P(OCH 3 ) 3 )37.2g, 1,2-dibromoethane (BrCH 2 CH 2 Br) 18.8g, catalyst (CH 3 ) 4NI 0.25g. Turn on the condensed water, heat and stir, and start to reflux when the temperature rises to about 120°C, continue heating, the temperature gradually rises to 170°C, and the degree of reflux decreases significantly. Continue the reaction, and when there is basically no reflux, keep the temperature at 180-190°C for 1 hour. Atmospheric distillation yielded 35.5 g of a colorless and transparent product with a total yield of 95.9%, among which the yield of tetramethyl 1,2-ethylenebisphosphonate was 86.5%.
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Abstract
The invention discloses a method for preparing a monophosphonate and biphosphonate mixed fire retardant, which comprises the following steps of: (1) heating tris phosphite and dihalide in the presence of a catalyst: (2) refluxing the mixture after the temperature rises to 110 to130 DEG C and continuously heating the refluxed mixture, wherein the optimal refluxing temperature of 120 DEG C; (3) allowing the refluxing speed to reduce obviously when the temperature is 160 and 180 DEG C, wherein the optimal temperature is 170 DEG C; (4) continuing a reaction, keeping the temperature between 170 and 200 DEG C to perform a reaction for 1 hour when the reflux phenomenon basically disappears, wherein the reaction is performed at 180 to190 DEG C optimally; (5) distilling the reacting product under normal pressure and filtering the distilled product to obtain a colorless transparent product. The total product yield of the monophosphonate and biphosphonate mixed fire retardant is over 90 percent; and the reaction time is shortened, the product has good color and luster, the acid value is low, the viscosity is low and no additional de-coloration treatment is required. Serving as the additive-type phosphine fire retardant, the monophosphonate and biphosphonate mixed fire retardant has higher performance. The monophosphonate and biphosphonate mixed fire retardant has the advantages of high economy, high product utilization efficiency, zero emission in a production process and environmental protection.
Description
technical field [0001] The invention relates to a preparation method of single and double mixed phosphonate flame retardants. Background technique [0002] Phosphonate is an additive flame retardant. Due to the existence of carbon-phosphorus bond, its chemical stability is enhanced. Only at very high temperature, the bond can be broken, so the flame retardant performance is durable. Bisphosphonate has the characteristics of high molecular weight, low volatility, hydrolysis resistance, solvent resistance, and good thermal stability. It can be widely used in flame retardancy of polymer materials such as polyolefins, polyesters, artificial fibers, and polyurethanes. Has good development prospects. [0003] There are three main synthetic methods reported in the literature at present: 1. The target product is obtained directly through polycondensation and Arbuzov rearrangement reaction of phosphite triester and dihalide; 2. Phosphorus trichloride, epichlorohydrin and triethylene...
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