Method of synthesizing ferrate
09682870 ยท 2017-06-20
Inventors
Cpc classification
C01G49/0081
CHEMISTRY; METALLURGY
International classification
Abstract
A method of synthesizing ferrate, which includes the steps of: (a) weighing and obtaining iron salts, activating agents, alkalinizing agents and oxidizing agents solution; (b) mixing uniformly the iron salts, the activating agents and the alkalinizing agents, heating to 30398 C. and maintaining for 1 min60 min to obtain a mixture; (c) adding the oxidizing agents solution to the mixture with an adding time of less than 10 minutes, then obtaining a precursor; and (d) natural cooling the precursor, then mixing the precursor with water and stirring evenly to obtain a final product of ferrate, wherein a volume ratio of the precursor and the water is 1:15. The method involves low power consumption, low temperature, low explosion risk, non-complicated steps and procedures, short synthetic time and high ferrate conversion efficiency. The method produces ferrate of high yield and good stability, and is suitable for producing ferrate composite pharmaceuticals in industrialized mass production.
Claims
1. A method of synthesizing ferrate composite pharmaceuticals, comprising the steps of: (a) weighing iron salts, activating agents, alkalinizing agents and oxidizing agents solution to obtain a molar ratio of iron salts and activating agents of 1:0.00110, a molar ratio of iron salts and alkalinizing agents of 1:220, a molar ratio of iron salts and oxidizing agents in the oxidizing agents solution of 1:0.110; (b) mixing said iron salts, said activating agents and said alkalinizing agents, then heating said iron salts, said activating agents and said alkalinizing agents after mixing to a temperature of 30 C.398 C. and maintaining said iron salts, said activating agents and said alkalinizing agents after heating for a time of 1 min60 min to obtain a mixture; (c) adding said oxidizing agents solution to said mixture for an adding time controlled at less than 10 minutes to obtain a precursor; and (d) natural cooling said precursor, then mixing said precursor with water and stirring to obtain a final product of ferrate composite pharmaceuticals, wherein a volume ratio of said precursor and said water is 1:15.
2. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein said iron salts in the step (a) is one or more selected from the group consisting of: ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate.
3. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein said activating agents in the step (a) is one or more selected from the group consisting of: potassium permanganate, potassium dichromate, potassium chlorate, persulfate and monopersulfate.
4. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein said alkalinizing agents in the step (a) is one or more selected from the group consisting of: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate.
5. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein said oxidizing agents solution in the step (a) is one or more selected from the group consisting of: potassium permanganate, potassium dichromate, hydrogen peroxide, ozone, sodium hypochlorite, potassium hypochlorite, potassium chlorate, perchlorate, persulfate and monopersulfate, wherein a concentration of said oxidizing agents solution is 0.1 mol/L3 mol/L.
6. The method of synthesizing ferrate composite pharmaceuticals according to claim 5, wherein said concentration of said oxidizing agents solution is 1.5 mol/L.
7. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein in the step (b), said temperature is 31 C.150 C.
8. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein in the step (b), said temperature is 151 C.397 C.
9. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein in the step (b), said time is 8 min10 min.
10. The method of synthesizing ferrate composite pharmaceuticals according to claim 1, wherein in the step (b), said time is 25 min30 min.
11. A method of synthesizing ferrate for producing ferrate composite pharmaceuticals in industrialized mass production, comprising the steps of: (a) weighing iron salts, activating agents, alkalinizing agents and oxidizing agents solution to obtain a molar ratio of iron salts and activating agents of 1:0.00110, a molar ratio of iron salts and alkalinizing agents of 1:220, a molar ratio of iron salts and oxidizing agents in the oxidizing agents solution of 1:0.110; (b) mixing said iron salts, said activating agents and said alkalinizing agents and then heating said iron salts, said activating agents and said alkalinizing agents after mixing to a temperature of 30 C.398 C.; (c) then maintaining said iron salts, said activating agents and said alkalinizing agents after the step (b) for a time of 1 min60 min to obtain a mixture; (d) adding said oxidizing agents solution to said mixture for an adding time controlled at less than 10 minutes to obtain a precursor; and (e) natural cooling said precursor, then mixing said precursor with water and stirring to obtain a final product of ferrate, wherein a volume ratio of said precursor and said water is 1:15, wherein a temperature for said method is between 30 C. and 398 C. and a processing time for said method is controlled to approximately less than 120 minutes, wherein a yield of said final product of ferrate is 60%95% and the maximum absorption peak in UV-Visible spectrum of said final product of ferrate is 525 nm, wherein said final product of ferrate is in liquid state.
12. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 11, wherein said iron salts in the step (a) is one or more selected from the group consisting of: ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate.
13. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 12, wherein said activating agents in the step (a) is one or more selected from the group consisting of: potassium permanganate, potassium dichromate, potassium chlorate, persulfate and monopersulfate, said alkalinizing agents in the step (a) is one or more selected from the group consisting of: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate, said oxidizing agents solution in the step (a) is one or more selected from the group consisting of: potassium permanganate, potassium dichromate, hydrogen peroxide, ozone, sodium hypochlorite, potassium hypochlorite, potassium chlorate, perchlorate, persulfate and monopersulfate, wherein a concentration of said oxidizing agents solution is 0.1 mol/L3 mol/L.
14. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 12, wherein in the step (b), said temperature is 31 C.150 C., wherein after the step (b), further comprises the step of: adding an additional amount of activating agents so as to increase a conversion efficiency of ferrate by 20%40%.
15. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 13, wherein in the step (b), said temperature is 31 C.150 C., wherein after the step (b), further comprises the step of: adding an additional amount of activating agents so as to increase a conversion efficiency of ferrate by 20%40%.
16. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 13, wherein in the step (b), said temperature is 151 C.397 C., wherein after the step (b), further comprises the step of: adding an additional amount of activating agents so as to increase a conversion efficiency of ferrate by 10%20%.
17. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 15, wherein in the step (c), said time is 8 min10 min, wherein said processing time for said method is approximately less than 60 minutes.
18. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 16, wherein in the step (c), said time is 8 min10 min, wherein said processing time for said method is approximately less than 60 minutes.
19. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 11, wherein in the step (a), said iron salts is ferrate nitrate, said activating agents is potassium dichromate and monopersulfate with a mass ratio of 1:4, said alkalinizing agents is potassium hydroxide, said oxidizing agents in said oxidizing agents solution is ozone, wherein in the step (b), said temperature is 40 C., wherein in the step (c), said time is 5 minutes, wherein said yield of said final product of ferrate is 8690%.
20. The method of synthesizing ferrate for producing ferrate composite pharmaceuticals according to claim 19, wherein a concentration of said oxidizing agents solution is 0.1 mol/L and said adding time is less than 0.5 minute, wherein said processing time for said method is approximately less than 30 minutes.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1)
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
(2) The present invention is further described in details with the accompanying drawings and embodiments. The following embodiments are shown and described for the purposes of illustrating the functional and structural principles of the present invention and is subject to change without departure from such principles. Therefore, this invention includes all modifications encompassed within the spirit and scope of the present invention.
Embodiment 1
(3) According to a method of synthesizing ferrate composite pharmaceutical of the preferred embodiment of the present invention, the process comprises the following steps:
(4) (a) Weight to obtain iron salts, activating agents, alkalinizing agents and oxidizing agents solution, where the molar ratio of iron salts and activating agents is 1:0.00110, the molar ratio of iron salts and alkalinizing agents is 1:220, the molar ratio of iron salts and oxidizing agents in the oxidizing agents solution is 1:0.110;
(5) (b) Mixing the iron salts, the activating agents and the alkalinizing agents, heating the iron salts, the activating agents and the alkalinizing agents to a temperature of 30398 C. and maintaining the iron salts, the activating agents and alkalinizing agents for a time of 1 min60 min to obtain a mixture;
(6) (c) Adding the oxidizing agents solution to the mixture in which an adding time is controlled at less than 10 minutes, and obtaining a precursor; and
(7) (d) Natural cooling the precursor, then mixing the precursor with water and stirring to obtain ferrate products, which is used as a ferrate composite pharmaceutical, where the volume ratio of the precursor and the water is 1:15.
(8) It is worth mentioning that the ferrate composite pharmaceutical produced by the method of the present invention can also be used for other purposes, such as drinking water treatment, wastewater treatment and etc.
(9) Preferably, in the step (d), the process of natural cooling is cooling to room temperature.
Embodiment 2
(10) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (a), the iron salts refer to a composition containing one or more of: ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate.
Embodiment 3
(11) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (a), the activating agents refers to one or more of: potassium permanganate, potassium dichromate, potassium chlorate, persulfate and monopersulfates.
Embodiment 4
(12) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (a), the alkalinizing agents refers to one or more of: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate.
Embodiment 5
(13) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (a), the oxidizing agents in the oxidizing solution refers to one or more of: potassium permanganate, potassium dichromate, hydrogen peroxide, ozone, sodium hypochlorite, potassium hypochlorite, potassium chlorate, perchlorate, persulfate and monopersulfate. The concentration of the oxidizing agents solution is 0.1 mol/L3 mol/L.
Embodiment 6
(14) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiments 1-5 except the followings: in step (a), the concentration of the oxidizing agents solution is 1.5 mol/L.
Embodiment 7
(15) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (b), the temperature is 31 C.150 C.
Embodiment 8
(16) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (b), the temperature is 151 C.397 C.
Embodiment 9
(17) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (b), the time is 8 min10 min.
Embodiment 10
(18) According to a method of synthesizing ferrate of this preferred embodiment of the present invention, all the steps and parameters are the same as that of embodiment 1 except the followings: in step (b), the time is 25 min30 min.
(19) The advantageous effect of the method of synthesizing ferrate of the present invention is tested and verified by the followings:
Embodiment 1
(20) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(21) (a) Weight to obtain 2.5 g of ferric nitrate, 0.5 g of potassium dichromate, 2.2 g of potassium hydroxide and 5 mL of 1.5 mol/L hydrogen peroxide solution;
(22) (b) Mixing the ferric nitrate, the potassium dichromate and the potassium hydroxide, heating the ferric nitrate, the potassium dichromate and the potassium hydroxide to a temperature of 300 C. and maintaining the ferric nitrate, the potassium dichromate and the potassium hydroxide for a time of 5 min to obtain a mixture;
(23) (c) Adding the 5 mL of hydrogen peroxide solution (1.5 mol/L) to the mixture in which an adding time is controlled at less than 0.5 minute, and obtaining a precursor; and
(24) (d) Natural cooling the precursor obtained, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 7375%.
Embodiment 2
(25) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(26) (a) Weight to obtain 2.0 g of ferric sulfate, 0.5 g of activating agent, 2.2 g of potassium hydroxide and 3 mL of 3 mol/L hydrogen peroxide solution, where the activating agent is a mixture of potassium persulfate and potassium permanganate of which the mass ratio of potassium persulfate and potassium permanganate is 4:1;
(27) (b) Mixing the ferric sulfate, the activating agent and the potassium hydroxide, heating the ferric sulfate, the activating agent and the potassium hydroxide to a temperature of 200 C. and maintaining for a time of 7.5 min to obtain a mixture;
(28) (c) Adding the 3 mL of hydrogen peroxide solution (3 mol/L) to the mixture in which an adding time is controlled at less than 0.5 minute, and obtaining a precursor; and
(29) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 9093%.
Embodiment 3
(30) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(31) (a) Weight to obtain 2.5 g of ferric nitrate, 0.5 g of activating agent, 2.2 g of potassium hydroxide and 5 mL of 2 mol/L sodium hypochlorite solution; where the activating agent is a mixture of potassium dichromate and potassium chlorate of which the mass ratio of potassium dichromate and potassium chlorate is 3:2;
(32) (b) Mixing the ferric nitrate, the activating agent and the potassium hydroxide obtained, heating the ferric nitrate, the activating agent and the potassium hydroxide to a temperature of 150 C. and maintaining the ferric nitrate, the activating agent and the potassium hydroxide for a time of 10 min to obtain a mixture;
(33) (c) Adding the 5 mL of sodium hypochlorite solution (2 mol/L) to the mixture in which an adding time is controlled at less than 0.5 minute, and obtaining a precursor; and
(34) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 8386%.
Embodiment 4
(35) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(36) (a) Weight to obtain 2.5 g of ferric nitrate, 0.5 g of activating agent, 2.2 g of potassium hydroxide and 5 mL of 1.5 mol/L perchloric acid solution, where the activating agent is a mixture of potassium dichromate and peroxydisulfates of which the mass ratio of potassium dichromate and peroxydisulfates is 2:3;
(37) (b) Mixing the ferric nitrate, the activating agent and the potassium hydroxide, heating the ferric nitrate, the activating agent and the potassium hydroxide to a temperature of 350 C. and maintaining the ferric nitrate, the activating agent and the potassium hydroxide for a time of 5 min to obtain a mixture;
(38) (c) Adding the 5 mL of perchloric acid solution (1.5 mol/L) to the mixture in which an adding time is controlled at less than 2 minute, and obtaining a precursor; and
(39) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 9093%.
Embodiment 5
(40) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(41) (a) Weight to obtain 2.5 g of ferric nitrate, 0.5 g of activating agent, 2.2 g of potassium hydroxide and 5 mL of 0.1 mol/L ozone solution, where the activating agent is a mixture of potassium dichromate and monopersulfate of which the mass ratio of potassium dichromate and monopersulfate is 1:4;
(42) (b) Mixing the ferric nitrate, the activating agent and the potassium hydroxide, heating the ferric nitrate, the activating agent and the potassium hydroxide to a temperature of 40 C. and maintaining the ferric nitrate, the activating agent and the potassium hydroxide for a time of 5 min to obtain a mixture;
(43) (c) Adding the 5 mL of ozone solution (0.1 mol/L) to the mixture in which an adding time is controlled at less than 0.5 minute, and obtaining a precursor; and
(44) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 8690%.
Embodiment 6
(45) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(46) (a) Weight to obtain 2.5 g of ferric chloride, 0.5 g of potassium permanganate, 2.2 g of potassium hydroxide and 5 mL of 2 mol/L potassium hypochlorite solution;
(47) (b) Mixing the ferric chloride, the potassium permanganate and the potassium hydroxide, heating the ferric chloride, the potassium permanganate and the potassium hydroxide to a temperature of 300 C. and maintaining the ferric chloride, the potassium permanganate and the potassium hydroxide for a time of 5 min to obtain a mixture;
(48) (c) Adding the 5 mL of potassium hypochlorite solution (2 mol/L) to the mixture in which an adding time is controlled at less than 1 minute, and obtaining a precursor; and
(49) (d) Natural cooling the precursor, then mixing the precursor with 10 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 9193%.
(50) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(51) (a) Weight to obtain 2.5 g of ferric chloride, 0.5 g of potassium dichromate, 2.2 g of potassium hydroxide and 5 mL of 1.5 mol/L hydrogen peroxide solution;
(52) (b) Mixing the ferric chloride, the potassium dichromate and the potassium hydroxide, heating the ferric chloride, the potassium dichromate and the potassium hydroxide to a temperature of 200 C. and maintaining the ferric chloride, the potassium dichromate and the potassium hydroxide for a time of 15 min to obtain a mixture;
(53) (c) Adding the 5 mL of hydrogen peroxide solution (1.5 mol/L) to the mixture in which an adding time is controlled at less than 0.5 minute, and obtaining a precursor; and
(54) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 8284%.
Embodiment 8
(55) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(56) (a) Weight to obtain 2.5 g of ferric chloride, 0.5 g of potassium dichromate, 2.2 g of sodium carbonate and 5 mL of 1.5 mol/L potassium persulfate solution;
(57) (b) Mixing the ferric chloride, the potassium dichromate and the sodium carbonate, heating the ferric chloride, the potassium dichromate and the sodium carbonate to a temperature of 200 C. and maintaining the ferric chloride, the potassium dichromate and the sodium carbonate for a time of 9 min to obtain a mixture;
(58) (c) Adding the 5 mL of potassium persulfate solution (1.5 mol/L) to the mixture in which an adding time is controlled at less than 2 minute, and obtaining a precursor; and
(59) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 8993%.
Embodiment 9
(60) According to a method of synthesizing ferrate composite pharmaceutical of this preferred embodiment of the present invention, the method comprises the following steps:
(61) (a) Weight to obtain 2.5 g of ferric nitrate, 0.5 g of potassium dichromate, 2.2 g of potassium hydroxide and 5 mL of 1.5 mol/L hydrogen peroxide solution;
(62) (b) Mixing the ferric nitrate, the potassium dichromate and the potassium hydroxide, heating the ferric nitrate, the potassium dichromate and the potassium hydroxide to a temperature of 390 C. and maintaining the ferric nitrate, the potassium dichromate and the potassium hydroxide for a time of 20 min to obtain a mixture;
(63) (c) Adding the 5 mL of hydrogen peroxide solution (1.5 mol/L) to the mixture in which an adding time is controlled at less than 5 minute, and obtaining a precursor; and
(64) (d) Natural cooling the precursor, then mixing the precursor with 5 mL of water and stirring to obtain ferrate products, which is a ferrate composite pharmaceutical, where a yield of the ferrate products is 7378%.
(65) One skilled in the art will understand that the embodiment of the present invention as shown in the drawings and described above is exemplary only and not intended to be limiting.
(66) It will thus be seen that the objects of the present invention have been fully and effectively accomplished. It embodiments have been shown and described for the purposes of illustrating the functional and structural principles of the present invention and is subject to change without departure from such principles. Therefore, this invention includes all modifications encompassed within the spirit and scope of the following claims.