Method for preparing melamine salt of pentaerypolyol phosphoric acid
View Patent ↗A method for preparing a melamine salt of pentaerypolyol phosphoric acid is provided. The method comprises the following steps of: ball milling a mixture of pentaerypolyol and phosphorus pentoxide (P 2 O 5 ) under a solvent-free reacting environment to obtain a pentaerypolyol phosphoric acid, and ball milling a mixture of a pentaerypolyol phosphoric acid and melamine without organic solvent reacting environment to obtain a melamine salt of pentaerypolyol phosphoric acid.
1. A catalyst-free method for preparing a melamine salt of pentaerypolyol phosphoric acid, comprising the steps of:
a. ball milling a first mixture comprised of pentaerypolyol and phosphorus pentoxide (P 2 O 5 ), which includes no catalyst, in a reacting environment which is free of solvent to obtain a pentaerypolyol phosphoric acid, wherein ball milling takes place in a ball mill used as a reactor; and
b. ball milling a second mixture comprised of said pentaerypolyol phosphoric acid and melamine, which includes no catalyst, in a reacting environment which is free of organic solvent, to obtain the melamine salt of pentaerypolyol phosphoric acid.
2. The catalyst-free method of claim 1 , wherein ball milling in step (a) proceeds at a temperature ranging from room temperature to 150° C.
3. The catalyst-free method of claim 1 , wherein the ball mill is preheated to a temperature of 110° C. for one half hour.
4. The catalyst-free method of claim 1 , wherein the pentaerypolyol is selected from the group consisting of 2,2-dimethyl-1,3-neopentyl glycol, 1,1,1-tris(hydroxymethyl)-ethane (tHME), pentaerythritol (PE) and dipentaerythritol (DPE).
5. The catalyst-free method of claim 1 , wherein the second mixture further comprises water.
6. The catalyst-free method of claim 1 , wherein ball milling in step (a) proceeds for a time ranging up to 6 hours.
7. The catalyst-free method of claim 6 , wherein ball milling in step (a) proceeds for a time ranging from 1 to 6 hours.
8. The catalyst-free method of claim 6 , wherein ball milling in step (a) proceeds for a time of 1 hour.
9. A catalyst-free method for preparing a melamine salt of pentaerypolyol phosphoric acid, comprising:
a. ball milling a first mixture comprised of pentaerypolyol and phosphorus pentoxide (P 2 O 5 ), which includes no catalyst, in a reacting environment which is free of solvent for six hours to obtain a pentaerypolyol phosphoric acid, wherein ball milling takes place in a ball mill used as a reactor; and
b. ball milling a second mixture comprised of said pentaerypolyol phosphoric acid and melamine which includes no catalyst, in a reacting environment which is free of organic solvent, to obtain the melamine salt of pentaerypolyol phosphoric acid.
10. The catalyst-free method of claim 9 , wherein ball milling in step (a) proceeds at a temperature ranging from room temperature to 150° C.
11. The catalyst-free method of claim 9 , wherein the ball mill is preheated to a temperature of 110° C. for one half hour.
12. The catalyst-free method of claim 9 , wherein the pentaerypolyol is selected from the group consisting of 2,2-dimethyl-1,3-neopentyl glycol, 1,1,1-tris(hydroxymethyl)-ethane (tHME), pentaerythritol (PE) and dipentaerythritol (DPE).
13. The catalyst-free method of claim 9 , wherein the second mixture further comprises water.
14. The catalyst-free method according to claim 1 , wherein the ball mill is preheated before the step of ball milling to a temperature ranging from 80 to 150° C.
15. The catalyst-free method according to claim 9 , wherein the ball mill is preheated before the step of ball milling to a temperature ranging from 80 to 150° C.