Preparation method for composite ferrate reagent

Abstract

A preparation method for a composite ferrate reagent. 1, Weigh raw materials; 2, evenly mix a ferric salt, an activating agent and an alkali maintaining agent and heat the mixture; 3, add an oxidant solution; and 4, cool and mix the solution with water. The technical problems of high energy consumption, low yield and poor ferrate product stability of the existing method for preparing ferrate are solved. The obtained product can be stably stored, and the yield of the ferrate reaches 60% to 95%.

Claims

1. A preparation method for ferrate composite agent, characterized in that, the preparation method for ferrate composite agent comprises the steps, in order, of: (1) weighing iron salt, activate agent, alkalinizing agent and oxidizing agent solution obtain a molar ratio of iron salt and activate agent of 1:0.00110, a molar ratio of iron salt and alkalinizing agent of 1:220, a molar ratio of iron salt and oxidizing agent in the oxidizing agent solution of 1:0.110; (2) mixing said iron salt, said activate agent and said alkalinizing agent obtained from the step (1) uniformly, heating said iron salt, said activate agent and said alkalinizing agent after mixing to a heating temperature of 150 C.390 C. and maintaining said iron salt, said activate agent and said alkalinizing agent after heating for a heating period of 5 min20 min, and obtaining a mixture; (3) adding said oxidizing agent solution from the step (1) to said mixture in the step (2), wherein an adding time is controlled below 10 minutes, then obtaining a precursor; and (4) cooling said precursor obtained from the step (3) naturally, then mixing said precursor with water according to a volume ratio of said precursor and said water of 1:15, stirring uniformly and obtaining the ferrate composite agent; wherein in the step (1), said activate agent is one or a combination of two or more selected from the group consisting of: potassium permanganate, potassium dichromate, potassium chlorate, persulfate and monopersulfate; and said oxidizing agent is one or a combination of two 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 agent solution is 0.1 mol/L3 mol/L.

2. The preparation method for ferrate composite agent according to claim 1, characterized in that, in the step (1), said iron salt is one or a combination of two or more selected from the group consisting of: ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate.

3. The preparation method for ferrate composite agent according to claim 1, characterized in that, in the step (1), said alkalinizing agent is one or a combination of two or more selected from the group consisting of: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate.

4. The preparation method for ferrate composite agent according to claim 1, characterized in that, said concentration of said oxidizing agent solution is 1.5 mol/L.

5. A preparation method for ferrate composite agent, consisting the steps, in order, of: (1) weighing iron salt, activate agent, alkalinizing agent and oxidizing agent solution obtain a molar ratio of iron salt and activate agent of 1:0.00110, a molar ratio of iron salt and alkalinizing agent of 1:220, a molar ratio of iron salt and oxidizing agent in the oxidizing agent solution of 1:0.110, wherein said activate agent is one or a combination of two or more selected from the group consisting of: potassium permanganate, potassium dichromate, potassium chlorate, persulfate and monopersulfate, wherein said oxidizing agent is one or a combination of two 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 agent solution is 0.1 mol/L3 mol/L; (2) mixing said iron salt, said activate agent and said alkalinizing agent obtained from the step (1) uniformly, heating said iron salt, said activate agent and said alkalinizing agent after mixing to a heating temperature of 150 C.390 C. and maintaining said iron salt, said activate agent and said alkalinizing agent after heating for a heating period of 5 min20 min, and obtaining a mixture; (3) adding said oxidizing agent solution from the step (1) to said mixture in the step (2), wherein an adding time is controlled below 10 minutes, then obtaining a precursor; and (4) cooling said precursor obtained from the step (3) naturally, then mixing said precursor with water according to a volume ratio of said precursor and said water of 1:15, stirring uniformly and obtaining the ferrate composite agent.

6. The preparation method for ferrate composite agent according to claim 5, wherein in the step (1), said iron salt is a divalent iron compound.

7. The preparation method for ferrate composite agent according to claim 5, wherein in the step (1), said iron salt is a trivalent iron compound.

8. The preparation method for ferrate composite agent according to claim 5, wherein in the step (1), said iron salt is one or a combination of the group consisting of a divalent iron compound or a trivalent iron compound.

9. The preparation method for ferrate composite agent according to claim 5, wherein in the step (1), said iron salt is one or a combination of two or more selected from the group consisting of: ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate.

10. The preparation method for ferrate composite agent according to claim 5, wherein in the step (1), said iron salt is one or a combination of two or more selected from the group consisting of: ferrous chloride, ferrous nitrate, and ferrous sulfate.

11. The preparation method for ferrate composite agent according to claim 5, wherein in the step (1), said alkalinizing agent is one or a combination of two or more selected from the group consisting of: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate.

12. The preparation method for ferrate composite agent according to claim 9, wherein in the step (1), said alkalinizing agent is one or a combination of two or more selected from the group consisting of: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate.

13. The preparation method for ferrate composite agent according to claim 5, wherein said concentration of said oxidizing agent solution is 1.5 mol/L.

14. The preparation method for ferrate composite agent according to claim 12, wherein said concentration of said oxidizing agent solution is 1.5 mol/L.

Description

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT

(1) The embodiment of the present invention as shown and described below is exemplary only and not intended to be limiting. This invention includes all combinations of different embodiments of the present invention.

(2) Preferred embodiment 1: According to a preparation method for ferrate composite agent of the preferred embodiment of the present invention, the method comprises the following steps:

(3) (1) weighing and obtaining iron salt, activate agent, alkalinizing agent and oxidizing agent solution, wherein a molar ratio of iron salt and activate agent is 1:0.00110, a molar ratio of iron salt and alkalinizing agent is 1:220, a molar ratio of iron salt and oxidizing agent in the oxidizing agent solution is 1:0.110;

(4) (2) mixing the iron salt, the activate agent and the alkalinizing agent obtained from the step (1) uniformly, heating to a heating temperature of 30 C.398 C. and maintaining for a heating period of 1 min60 min, and obtaining a mixture;

(5) (3) adding the oxidizing agent solution from the step (1) to the mixture in the step (2), wherein an adding time is controlled below 10 minutes, then obtaining a precursor; and

(6) (4) cooling the precursor obtained from the step (3) naturally, then mixing the precursor with water according to a volume ratio of the precursor and the water of 1:15, stirring uniformly and obtaining the ferrate composite agent.

(7) Preferred embodiment 2: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (1), the iron salt is one or a combination of two or more of the followings: ferric chloride, ferrous chloride, ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate. All others are the same as that of the above preferred embodiment 1.

(8) Preferred embodiment 3: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (1), the activate agent is one or a combination of two or more of the followings: potassium permanganate, potassium dichromate, potassium chlorate, persulfate and monopersulfate. All others are the same as that of the above preferred embodiment 1.

(9) Preferred embodiment 4: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (1), the alkalinizing agent is one or a combination of two or more of the followings: sodium hydroxide, sodium carbonate, sodium bicarbonate, potassium hydroxide, potassium bicarbonate and potassium carbonate. All others are the same as that of the above preferred embodiment 1.

(10) Preferred embodiment 5: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (1), the oxidizing agent is one or a combination of two or more of the followings: potassium permanganate, potassium dichromate, hydrogen peroxide, ozone, sodium hypochlorite, potassium hypochlorite, potassium chlorate, perchlorate, persulfate and monopersulfate. The concentration of the oxidizing agent solution is 0.1 mol/L3 mol/L. All others are the same as that of the above preferred embodiment 1.

(11) Preferred embodiment 6: The difference between this preferred embodiment and one of the above preferred embodiment 1-5 is that: in the step (1), the concentration of the oxidizing agent solution is 1.5 mol/L. All others are the same as that of one of the above preferred embodiment 1-5.

(12) Preferred embodiment 7: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (2), the heating temperature is 31 C.150 C. All others are the same as that of the above preferred embodiment 1.

(13) Preferred embodiment 8: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (2), the heating temperature is 151 C.397 C. All others are the same as that of the above preferred embodiment 1.

(14) Preferred embodiment 9: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (2), the heating period is 8 min10 min. All others are the same as that of the above preferred embodiment 1.

(15) Preferred embodiment 10: The difference between this preferred embodiment and the above preferred embodiment 1 is that: in the step (2), the heating period is 25 min30 min. All others are the same as that of the above preferred embodiment 1.

(16) The following exemplary embodiments are used to test and verify the advantageous effect of the present invention:

Exemplary Embodiment 1

(17) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(18) (1) Weighing and obtaining 2.5 g ferric nitrate, 0.5 g potassium dichromate, 2.2 g potassium hydroxide and 5 mL hydrogen peroxide solution (concentration: 1.5 mol/L);

(19) (2) Mixing the ferric nitrate, the potassium dichromate and the potassium hydroxide obtained from step (1) uniformly, heating to 300 C., maintaining for 5 min and obtaining a mixture;

(20) (3) Adding the 5 mL hydrogen peroxide solution (concentration 1.5 mol/L) obtained from the step (1) to the mixture obtained from the step (2), controlling an adding time to less than 0.5 minute, and obtaining a precursor; and

(21) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 7375%.

Exemplary Embodiment 2

(22) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(23) (1) Weighing and obtaining 2.0 g ferric sulfate, 0.5 g activate agent, 2.2 g potassium hydroxide and 5 mL hydrogen peroxide solution (concentration 3 mol/L), where the activate agent is a mixture of potassium persulfate and potassium permanganate of which the mass ratio of potassium persulfate and potassium permanganate is 4:1;

(24) (2) Mixing the ferric sulfate, the activate agent and the potassium hydroxide obtained from step (1) uniformly, heating to 200 C., maintaining for 7.5 min and obtaining a mixture;

(25) (3) Adding the 5 mL hydrogen peroxide solution (concentration 3 mol/L) obtained from step (1) to the mixture obtained from the step (2), controlling an adding time to less than 0.5 minute, and obtaining a precursor; and

(26) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 9093%.

Exemplary Embodiment 3

(27) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(28) (1) Weighing and obtaining 2.5 g ferric nitrate, 0.5 g activate agent, 2.2 g potassium hydroxide and 5 mL sodium hypochlorite solution (concentration 2 mol/L), where the activate agent is a mixture of potassium dichromate and potassium chlorate at a mass ratio of 3:2;

(29) (2) Mixing the ferric nitrate, the activate agent and the potassium hydroxide obtained from step (1) uniformly, heating to 150 C., maintaining for 10 min and obtaining a mixture;

(30) (3) Adding the 5 mL sodium hypochlorite solution (2 mol/L) obtained from the step (1) to the mixture obtained from the step (2), controlling an adding time to less than 0.5 minute and obtaining a precursor; and

(31) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 8386%.

Exemplary Embodiment 4

(32) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(33) (1) Weighing and obtaining 2.5 g ferric nitrate, 0.5 g activate agent, 2.2 g potassium hydroxide and 5 mL perchloric acid solution (1.5 mol/L), where the activate agent is a mixture of potassium dichromate and peroxydisulfates at a mass ratio of 2:3;

(34) (2) Mixing the ferric nitrate, the activate agent and the potassium hydroxide obtained from step (1) uniformly, heating to 350 C., maintaining for 5 min and obtaining a mixture;

(35) (3) Adding the 5 mL perchloric acid solution (1.5 mol/L) obtained from step (1) to the mixture obtained from the step (2), controlling an adding time to less than 2 minute, and obtaining a precursor; and

(36) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 9093%.

Exemplary Embodiment 5

(37) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(38) (1) Weighing and obtaining 2.5 g ferric nitrate, 0.5 g activate agent, 2.2 g potassium hydroxide and 5 mL ozone solution (concentration 0.1 mol/L), where the activate agent is a mixture of potassium dichromate and monopersulfate at a mass ratio of 1:4;

(39) (2) Mixing the ferric nitrate, the activate agent and the potassium hydroxide obtained from step (1) uniformly, heating to 40 C., maintaining for 5 min and obtaining a mixture;

(40) (3) Adding the 5 mL ozone solution (0.1 mol/L) obtained from step (1) to the mixture obtained the step (2), controlling an adding time to less than 0.5 minute and obtaining a precursor; and

(41) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 8690%.

Exemplary Embodiment 6

(42) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(43) (1) Weighing and obtaining 1.5 g ferric chloride, 0.5 g potassium permanganate, 2.2 g potassium hydroxide and 5 mL potassium hypochlorite solution (concentration 2 mol/L);

(44) (2) Mixing the ferric chloride, the potassium permanganate and the potassium hydroxide obtained from step (1) uniformly, heating to 300 C., maintaining for 5 min and obtaining a mixture;

(45) (3) Adding the 5 mL potassium hypochlorite solution (2 mol/L) obtained from step (1) to the mixture obtained from the step (2), controlling an adding time to less than 1 minute and obtaining a precursor; and

(46) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 10 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 9193%.

Exemplary Embodiment 7

(47) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(48) (1) Weighing and obtaining 2.5 g ferric chloride, 0.5 g potassium dichromate, 2.2 g potassium hydroxide and 5 mL hydrogen peroxide solution (concentration 1.5 mol/L);

(49) (2) Mixing the ferric chloride, the potassium dichromate and the potassium hydroxide obtained from step (1) uniformly, heating to 200 C., maintaining for 15 min and obtaining a mixture;

(50) (3) Adding the 5 mL hydrogen peroxide solution (1.5 mol/L) obtained from step (1) to the mixture obtained from the step (2), controlling an adding time to less than 0.5 minute and obtaining a precursor; and

(51) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 8284%.

Exemplary Embodiment 8

(52) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(53) (1) Weighing and obtaining 2.5 g ferric chloride, 0.5 g potassium dichromate, 2.2 g sodium carbonate and 5 mL potassium persulfate solution (1.5 mol/L);

(54) (2) Mixing the ferric chloride, the potassium dichromate and the sodium carbonate obtained from the step (1) uniformly, heating to 200 C., maintaining for 9 min and obtaining a mixture;

(55) (3) Adding the 5 mL potassium persulfate solution (1.5 mol/L) obtained from step (1) to the mixture obtained from the step (2), controlling an adding time to less than 2 minute and obtaining a precursor; and

(56) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 8993%.

Exemplary Embodiment 9

(57) According to a preparation method for ferrate composite agent of this exemplary embodiment of the present invention, the method comprises the following steps:

(58) (1) Weighing and obtaining 2.5 g ferric nitrate, 0.5 g potassium dichromate, 2.2 g potassium hydroxide and 5 mL hydrogen peroxide solution (concentration 1.5 mol/L);

(59) (2) Mixing the ferric nitrate, the potassium dichromate and the potassium hydroxide obtained from step (1) uniformly, heating to 390 C., maintaining for 20 min and obtaining a mixture;

(60) (3) Adding the 5 mL hydrogen peroxide solution (1.5 mol/L) obtained from step (1) to the mixture obtained from the step (2), controlling an adding time to less than 5 minute and obtaining a precursor; and

(61) (4) cooling the precursor obtained from step (3) naturally, then mixing the precursor with 5 mL water, stirring uniformly and obtaining the ferrate composite agent with a yield of 7378%.