CN103121718B

CN103121718B - Method for preparing X-shaped ammonium octamolybdate

Info

Publication number: CN103121718B
Application number: CN201310086834.4A
Authority: CN
Inventors: 唐军利
Original assignee: Jinduicheng Molybdenum Co Ltd
Current assignee: Jinduicheng Molybdenum Co Ltd
Priority date: 2013-03-19
Filing date: 2013-03-19
Publication date: 2014-10-01
Anticipated expiration: 2033-03-19
Also published as: CN103121718A

Abstract

The invention discloses a method for preparing X-shaped ammonium octamolybdate. The method comprises the following steps: (1) boiling an ammonia water solution with the pH value of 8.5 to 9.0, maintaining the boiling state, adding molybdenum trioxide into the ammonia water solution under a stirring condition until the pH value of the solution reaches 3.5 to 4.0, and stirring for 2 to 3 hours under a temperature maintaining condition; and (2) cooling the solution with the maintained temperature under the stirring condition until the temperature reaches 60 to 65 DEG C, stirring for 1 to 2 hours under the temperature maintaining condition, and cooling, filtering and drying, thereby obtaining the X-shaped ammonium octamolybdate. According to the method, the molybdenum trioxide is directly added into the ammonia water solution and can perform a polymerization reaction during the ammonia dissolving process, so that the solution is acidized; and therefore, by strictly regulating and controlling the pH value, the X-shaped ammonium octamolybdate is generated in a specific pH value range. The method is simple in process and easy to operate. The prepared X-shaped ammonium octamolybdate has stable ingredients.

Description

A kind of method of preparing X-type ammonium octamolybdate

Technical field

The invention belongs to chemical technology field, be specifically related to a kind of method of preparing X-type ammonium octamolybdate.

Background technology

At present molybdenum compounds as anti-flaming smoke-inhibiting agent research in China still in the starting stage, the inorganic smoke inhibition fire retardant that ammonium octamolybdate (AOM) is excellent performance, market potential is huge.Ammonium octamolybdate is added in PVC goods, and at the PVC thermolysis initial stage, ammonium octamolybdate can promote intermolecular crosslinking reaction Formed compound, increases into carbon amount, improves oxygen index, reduces combustible components, reduces raw cigarette speed and density, presses down cigarette object thereby reach.In addition, aspect powder processing, ammonium octamolybdate is because of its fine size, good dispersity, prepares molybdenum powder, the thin feature that has himself aspect brilliant of ultrafine molybdenum powder, molybdenum especially in the reduction of roasting knot, is usually used in preparing the molybdenum powder of Ultra-fine.

Ammonium octamolybdate has multiple isomers: α-AOM, β-AOM, γ-AOM and X-AOM.X-AOM Raman spectrum characteristic peak 953-995cm ^-1, 946-948cm ^-1, 796-798cm ^-1, at the anti-flaming smoke-inhibiting agent of cable sheathing, electric wire foreskin and fiber optic materials, its smoke suppressing effect is good, applies more and more extensive.X-AOM ingot is hard, purity is high, yield is high, can be well mixing with macromolecular material.

Prepare at present ammonium octamolybdate and generally adopt solubility molybdic acid ammonium (ammonium dimolybdate or Ammonium Heptamolybdate) and molybdic oxide, in the aqueous solution, react and make (as: CN100469703C, CN102060329A, US4762700, US6235261), preparation technology is more complicated, and its principle is:

4NH ₄ ⁺+2Mo ₂O ₇ ^2－+4MoO ₃=(NH ₄) ₄Mo ₈O ₂₆↓

Or 12NH ₄ ⁺+ 2Mo ₇o ₂₄ ^6-+ 10MoO ₃=3 (NH ₄) ₄mo ₈o ₂₆↓.

Summary of the invention

Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of method of preparing X-type ammonium octamolybdate is provided.The method directly adds molybdenum oxide in ammoniacal liquor, utilizes molybdenum oxide self polymerization reaction take place in the molten process of ammonia, and makes solution acidifying, by strict regulation and control pH value, within the scope of specific pH value, generate X-type ammonium octamolybdate, technique is simple, easily operation, the X-type ammonium octamolybdate stable components making.

For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of preparing X-type ammonium octamolybdate, it is characterized in that, and the method comprises the following steps:

Step 1, the ammonia soln that is 8.5～9.0 by pH value boil, keep boiling state, and under agitation condition, be 3.5～4.0 to adding molybdic oxide in ammonia soln to the pH value of solution, insulated and stirred 2h～3h; The speed that adds of described molybdic oxide is to keep pH to decline 0.6～1 in every ten minutes; In described stirring and insulated and stirred process, all keeping the solid-to-liquid ratio of solution by adding water is 1: 3～5;

Step 2, until in step 1 insulation after solution under agitation condition, be cooled to 60 DEG C～65 DEG C after insulated and stirred 1h～2h, cooled and filtered, dry, obtain X-type ammonium octamolybdate.

A kind of above-mentioned method of preparing X-type ammonium octamolybdate, the pH value of ammonia soln described in step 1 is 8.7.

A kind of above-mentioned method of preparing X-type ammonium octamolybdate is 3.8 to adding molybdic oxide to the pH value of solution in ammonia soln described in step 1 under agitation condition.

A kind of above-mentioned method of preparing X-type ammonium octamolybdate, the speed that adds of molybdic oxide described in step 1 is to keep pH to decline 0.8 in every ten minutes.

The present invention compared with prior art has the following advantages: the present invention directly adds molybdenum oxide in ammoniacal liquor, utilize molybdenum oxide self polymerization reaction take place in the molten process of ammonia, and make solution acidifying, by strict regulation and control pH value, within the scope of specific pH value, generate X-type ammonium octamolybdate, technique is simple, easily operation, the X-type ammonium octamolybdate stable components making.

Below by drawings and Examples, technical scheme of the present invention is described in further detail.

Brief description of the drawings

Fig. 1 is the Raman collection of illustrative plates of the X-type ammonium octamolybdate prepared of the embodiment of the present invention 1.

Fig. 2 is the Raman collection of illustrative plates of the X-type ammonium octamolybdate prepared of the embodiment of the present invention 2.

Fig. 3 is the Raman collection of illustrative plates of the X-type ammonium octamolybdate prepared of the embodiment of the present invention 3.

Embodiment

Embodiment 1

Step 1, the ammonia soln that is 8.5 by pH value boil, keep boiling state, and under agitation condition, be 3.5 to adding molybdic oxide in ammonia soln to the pH value of solution, insulated and stirred 2h; The speed that adds of described molybdic oxide is to keep pH to decline 1 in every ten minutes; In described stirring and insulated and stirred process, all keep the solid-to-liquid ratio of solution to be 1 by adding water: 5(solid-to-liquid ratio refers to the mass ratio of solid matter and liquid in solution);

Step 2, until in step 1 insulation after solution under agitation condition, be cooled to 65 DEG C after insulated and stirred 1h, cooled and filtered, dry, obtain X-type ammonium octamolybdate.

X-type ammonium octamolybdate prepared by the present embodiment carries out Raman spectrum detection, the result obtaining as shown in Figure 1, as can be seen from the figure, 796cm ^-1there is highest peak in place, is X-AOM(X type ammonium octamolybdate) characteristic peak, prove that the product preparing is X-type ammonium octamolybdate.

Embodiment 2

Step 1, the ammonia soln that is 8.7 by pH value boil, keep boiling state, and under agitation condition, be 3.8 to adding molybdic oxide in ammonia soln to the pH value of solution, insulated and stirred 2.5h; The speed that adds of described molybdic oxide is to keep pH to decline 0.8 in every ten minutes; In described stirring and insulated and stirred process, all keep the solid-to-liquid ratio of solution to be 1 by adding water: 4(solid-to-liquid ratio refers to the mass ratio of solid matter and liquid in solution);

Step 2, until in step 1 insulation after solution under agitation condition, be cooled to 62 DEG C after insulated and stirred 1.5h, cooled and filtered, dry, obtain X-type ammonium octamolybdate.

X-type ammonium octamolybdate prepared by the present embodiment carries out Raman spectrum detection, the result obtaining as shown in Figure 2, as can be seen from the figure, 796cm ^-1there is highest peak in place, is X-AOM(X type ammonium octamolybdate) characteristic peak, prove that the product preparing is X-type ammonium octamolybdate.

Embodiment 3

Step 1, the ammonia soln that is 9.0 by pH value boil, keep boiling state, and under agitation condition, be 4.0 to adding molybdic oxide in ammonia soln to the pH value of solution, insulated and stirred 3h; The speed that adds of described molybdic oxide is to keep pH to decline 0.6 in every ten minutes; In described stirring and insulated and stirred process, all keep the solid-to-liquid ratio of solution to be 1 by adding water: 3(solid-to-liquid ratio refers to the mass ratio of solid matter and liquid in solution);

Step 2, until in step 1 insulation after solution under agitation condition, be cooled to 60 DEG C after insulated and stirred 2h, cooled and filtered, dry, obtain X-type ammonium octamolybdate.

X-type ammonium octamolybdate prepared by the present embodiment carries out Raman spectrum detection, the result obtaining as shown in Figure 3, as can be seen from the figure, 796cm ^-1there is highest peak in place, is X-AOM(X type ammonium octamolybdate) characteristic peak, prove that the product preparing is X-type ammonium octamolybdate.

The above; it is only preferred embodiment of the present invention; not the present invention is done to any restriction, every any simple modification of above embodiment being done according to invention technical spirit, change and equivalent structure change, and all still belong in the protection domain of technical solution of the present invention.

Claims

1. a method of preparing X-type ammonium octamolybdate, is characterized in that, the method comprises the following steps:

Step 1, the ammonia soln that is 8.7 by pH value boil, keep boiling state, and under agitation condition, be 3.5～4.0 to adding molybdic oxide in ammonia soln to the pH value of solution, insulated and stirred 2h～3h; The speed that adds of described molybdic oxide is to keep pH to decline 0.6～1 in every ten minutes; In described stirring and insulated and stirred process, all keeping the solid-to-liquid ratio of solution by adding water is 1: 3～1: 5;

2. a kind of method of preparing X-type ammonium octamolybdate according to claim 1, is characterized in that, described in step 1, under agitation condition, is 3.8 to adding molybdic oxide to the pH value of solution in ammonia soln.

3. a kind of method of preparing X-type ammonium octamolybdate according to claim 1, is characterized in that, the speed that adds of molybdic oxide described in step 1 is to keep pH to decline 0.8 in every ten minutes.