Phosphorus-containing flame-retardant citrate PVC plasticizer and preparation method thereof
A technology of citrate and citrate, which is applied in the field of phosphorus-containing flame-retardant citrate PVC plasticizer and its preparation, can solve the problem of phosphate esters being easy to decompose, burn, and volatile citrate plasticizers and other problems, to achieve the effect of high polar bond content, reduced dependence, and excellent plasticizing performance
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Embodiment 1
[0027] Catalytic esterification of citric acid and hydroxymethyl phosphate in the first step: a certain amount of 100g citric acid, 256g dimethyl hydroxymethyl phosphate and 3.5g phosphotungstic acid were added to a room equipped with a stirrer, a water separator, a thermometer and nitrogen. A 1000ml four-necked flask was then introduced into nitrogen (5L / min) to start the stirring and heating reaction, and the reaction temperature was controlled to 130-160°C to carry out the esterification reaction. The reaction was carried out for 6.5h and the acid value was 3.72mg / g.
[0028] The second step is to recover phosphate under reduced pressure: control the temperature at 160 ° C and the degree of vacuum at -0.098MPa, carry out reduced pressure recovery of hydroxymethyl phosphate, when the recovered dimethyl hydroxymethyl phosphate reaches 14g, break the vacuum by nitrogen , the recovery of dimethyl hydroxymethyl phosphate ends.
[0029] The third step is neutralizing and washing:...
Embodiment 2
[0032] The first step of catalytic esterification of citric acid and hydroxymethyl phosphate: a certain 100g of citric acid, 298g of dimethyl hydroxymethyl phosphate and 5g of methanesulfonic acid were added to a room equipped with a stirrer, a water separator, a thermometer and nitrogen. A 1000ml four-necked flask was then introduced into nitrogen (5L / min) to start the stirring and heating reaction, and the reaction temperature was controlled at 130-160°C to carry out the esterification reaction. The reaction was carried out for 5.5h and the acid value was 3.15mg / g.
[0033] The second step is to recover phosphate under reduced pressure: control the temperature at 150-160°C and the degree of vacuum at -0.098MPa, carry out reduced pressure recovery of hydroxymethyl phosphate, and when the recovered hydroxymethyl phosphate reaches 56g, break the vacuum by nitrogen , the recovery of dimethyl hydroxymethyl phosphate ends.
[0034] The third step is neutralization and washing: coo...
Embodiment 3
[0037] The first step of catalytic esterification of citric acid and hydroxymethyl phosphate: a certain amount of 100g citric acid, 320g hydroxymethyl diethyl phosphate and 10g sulfamic acid methanesulfonic acid are added to a device equipped with a stirrer, a water separator and a thermometer. and nitrogen in a 1000ml four-necked flask, then introduce nitrogen (5L / min) to start the stirring and heating reaction, control the reaction temperature to 130-160℃, carry out esterification reaction, the reaction is carried out for 4.5h, and the acid value is 4.26mg / g, esterification the end of the reaction;
[0038]The second step is to recover phosphate under reduced pressure: control the temperature at 150-160°C and the degree of vacuum at -0.098MPa, perform reduced pressure recovery of hydroxymethyl phosphate, and when the recovered hydroxymethyl phosphate reaches 54g, break the vacuum by nitrogen , the recovery of hydroxymethyl diethyl phosphate ends.
[0039] The third step is ...
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