JPS60123578A - Manufacture unit for fluorescent substance - Google Patents

Abstract

PURPOSE:To provide titled unit capable of achieving significant energy conservation leading to reduction in production cost, by making an inert gas flow through the proximity of the exit of furnace into said furnace in the opposite direction to the moving direction of the calcinating material to effect higher thermal utilization as well as increased retention of the gas within the furnace. CONSTITUTION:Prior to the calcination of fluorescent substance, an inert gas e.g. N2, Ar, etc., is made to flow through ejection mouth 12 into the exit 3 in furnace 1, that is, in the opposite direction to the moving direction of vessels 8 on conveyor 6, using pressure pump 13 in gas introduction unit 11, to effect higher atmospheric pressure in cooling zone C; said inert gas introduction being performed continuously throughout the process. Following that, a feedstock mixture for the manufacture of fluorescent substance is filled in the vessels 8, which are mounted on the conveyor 6, being successively conveyed stepwise and continuously from inlet 2 to the exit 3 within the furnace 1 to carry out calcination.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention is directed to an apparatus for producing, for example, a five-day phosphor by firing an octoday phosphate phosphor.

[Technical background of the invention]

In general, helophosphate phosphor 9'c, calcium helophosphate phosphor, etc. are manufactured using an apparatus as shown in FIG. In Fig. 1 (al), (11 is a furnace body, and this furnace body (1) is hollow and elongated in the horizontal direction from the inlet part (2) to the outlet part (3). 3)
is open. In addition, gas exhaust ports +4] (5) are provided at the top of the inlet (2) side and outlet (3) side of the furnace body (1). A transfer body (6) is arranged, and this transfer body 16) is moved from the inlet part (2) to the outlet part (3) by means of a hydraulic pusher device (7).
At the same time, a refractory firing container (8) is placed on the transfer body (6) and moved.

Inside the furnace body 111, there is a preheating zone (4) where the temperature gradually increases from the inlet section (2) to the outlet section (3) at a firing temperature of 5 and a firing time as shown in Fig. 1. The firing zone (B) has a constant high temperature state, and the cooling zone 0 where the temperature gradually decreases.The phosphor synthetic material is filled into the container (8) and gradually moved from the inlet part (2) to the outlet part (3). It is set to 5 and moves continuously.

For example, in the production of calcium herophosphate phosphors, raw materials such as calcium phosphate, calcium carbonate, calcium fluoride, antimony trioxide, manganese carbonate, antimony chloride, or calcium chloride are generally thoroughly mixed. The container (8) filled with the synthetic material is placed on the transfer body (6) and transferred from the inlet part (2) to the outlet part (3) in the furnace body (1). ). Along with this transfer, the synthetic material filled in the container (8) is first decomposed in the preheating area (5), and the matrix of the phosphor (5Ca5(PO4)2-Ca(F
, C))2. Calcium apatite) is formed.

The decomposed gas generated during this decomposition is each gas exhaust port +4]
(Ejected from 51.

Next, an activator (Sb, Sb,
Dumping of Mn) into the matrix takes place, and a large amount of antimony chloride (Sbcl,
) The generation (synthesis) of the phosphor is completed in a gas atmosphere.

In this step, the firing container (8) is moved stepwise and continuously while maintaining an dwell time of 1.5 hours in the preheating zone and 1.5 hours in the firing zone.

[Problems with background technology]

However, in the above five methods, the vapor pressure of the cracked gas (H2O, CO2, etc.) generated in the preheating zone (A) is
) in the cooling zone (
This has the disadvantage that it flows into the phosphor and adheres to the surface of the produced phosphor (the surface of the container (8)), reducing the luminous efficiency of the phosphor.

In addition, antimony chloride (Sh
Since the vapor pressure of the gas (Cl,) is higher than that of the cooling zone (O) and the temperature is high, most of the steam (gas) escapes from the cooling zone (C) to the outside of the furnace body (1), forming antimony chloride (F3bC1,
) There is a problem that cannot be ignored in terms of manufacturing cost: lowering the gas concentration worsens the production of phosphor and also significantly lowers the thermal efficiency within the furnace body 11).

Furthermore, in the vicinity of the outlet (3) of the furnace body (1), some of the external air (02) flows into the cooling zone (0), and the activator is oxidized (MrL-+MrL) due to the high temperature of the surface of the phosphor. This causes the surface to be colored pink.Thus, the colored material significantly reduces the luminous output and cannot be used as a phosphor.Therefore, the production efficiency of the phosphor is reduced.

[Purpose of the invention]

The present invention has been made in view of the above-mentioned points, and improves the discharge and maintenance of the gas generated in each area, increases the luminous efficiency of the phosphor, and improves the efficiency of utilizing the heat amount in the furnace. The aim is to increase the

[Summary of the invention]

The present invention provides a furnace body that performs firing while moving a phosphor synthetic material filled in a fire-resistant firing container that is hollow and elongated from an inlet to an outlet. , an inert gas introducing device is provided at the outlet of the furnace body and introduces an inert gas near the outlet of the furnace body in a direction opposite to the moving direction of the phosphor synthetic material. It is something.

[Embodiments of the invention]

Hereinafter, one embodiment of the present invention will be described with reference to Fig. 2.

The device shown in Figure 2 (α) is also hollow and elongated in the horizontal direction from the inlet part (2) to the outlet part (3), and the outlet part (3) is open, similar to the device shown in Figure 1. Furnace body (1), inlet part (2) and gas exhaust port +41 on the upper part of the outlet part +31 side
(51, transport body (6), hydraulic pusher device (7),
It has the structure of a container (8) filled with a fluorescent synthetic material, and the gas exhaust port (5) at the upper part on the exit part (3) side is a gas pressure adjustment port that can be opened and closed freely.

Further, an inert gas introducing device all is provided at the outlet portion +31 of the furnace body (1). This inert gas introduction device uu is provided with an inert gas outlet lI21 at the upper and lower part of the outlet part (3),
One of these inert gas jet ports is connected to an inert gas source via a pressurizing pump G31. Also, heat generating elements Q41 are disposed at the upper and lower parts of the furnace body tll.

The inside of the furnace body (11) is a preheating area where the temperature gradually rises from the inlet (2) to the outlet A (3) at a firing temperature and firing time as shown in Figure 2. The firing zone (6) is at a high temperature, and the cooling zone (Ω) where the temperature gradually decreases.
However, compared to the device shown in Fig. 1, the preheating zone and the cooling zone are made larger.

Then, before firing the phosphor, inert gas such as nitrogen (N2) gas or argon (A?-) gas is injected into the inert gas introducing device [1] Therefore, the inert gas outlet (21) is placed on the outlet part (3) side in the furnace body 111, that is, the transfer body 1
6) in the direction opposite to the direction of movement of the container (8);
The air pressure in the cooling zone Ω is increased, and this inert gas is continuously introduced during the work.

For example, in the production of halophosphate phosphors, calcium phosphate (CaHPQ4), calcium carbonate (CjICo), calcium fluoride (CaF2), etc.
, calcium chloride (CaCl2) or ammonium chloride (NH4C1), antimony trioxide (8A20s
), manganese carbonate (btnco, ) raw materials are fully mixed into a container (8), and as in the past, the container (8) filled with this synthetic material is placed on the transfer body (6). Place it in the furnace body (1) from the inlet part (2) to the outlet part (3).
) are transferred step by step and continuously. Thereby, the synthetic material filled in the container (8) is heated in the preheating area (A
), the material decomposes and a phosphor matrix is formed.
In the firing zone (B), the activator is dapied to the matrix in an atmosphere of antimony chloride (ShC15) gas generated from the material, and in the cooling zone (B), the phosphor is dumped in a large amount of antimony chloride (S5cz) gas atmosphere. The generation (synthesis) of is completed.

At this time, as described in step 5 above, inert gas is introduced from near the outlet (3) of the furnace body (1) in the opposite direction to the moving direction of the container (81) to increase the pressure in the cooling zone (C). As a result, the decomposed gas generated in the preheating zone (4) is sufficiently discharged from the gas exhaust port +41 on the inlet section (2) side.Also, in this preheating zone, it takes nearly twice as much time as before. , complete decomposition of synthetic materials and elimination of decomposition gases.

In addition, antimony chloride (Sb, Cl,) gas, which is necessary for the production of phosphor and is generated in the firing zone (3), is reliably retained by the gas curtain effect of the inert gas, and is kept in the firing zone (B) and the cooling zone O. Maintain high concentration. Note that the vapor pressure of the 7th chloride (SbC15) gas, which increases stepwise, is maintained at a predetermined pressure by adjusting the gas exhaust port (5) as a gas pressure adjustment port.

In addition, in cooling zone 0, antimony chloride (SbcA',
) gas is sufficiently filled, and air from outside the furnace body (11) is blocked off with inert gas in the vicinity of the outlet +31, eliminating contact with air (02) and preventing the phosphor from coming into contact with the air (02). It can prevent the formation and oxidation of the activator and increase the luminous efficiency of the phosphor.In addition, the cooling zone (Q) has a sufficiently long transport time together with the presence of an inert gas, so the exit section (3)
The temperature drops to near room temperature, compared to about 500C in the conventional case, and the generated phosphor comes out from the outlet (3) in a stable state.

During actual work, for example, if the furnace body (1) has a total length of 15.6 m and a height of 1.117 m, inert gas of 110001/A is always flowed in, and the firing container (8) filled with synthetic material is transferred. C. is moved stepwise and continuously at a rate of 900 seconds/vessel IP by means of the body (6). Then, in the preheating area prisoner, it takes one hour to itch, which is almost twice as long as before.
Thoroughly decompose materials and remove decomposed gases.

Next, an example of a mixed material will be shown.

Material Weight J) Calcium phosphate CaHPO41D 7, OO calcium carbonate CcLCOs 52, 70 Calcium fluoride CcLF29゜75 Calcium chloride CaC121゜20 Antimony oxide 5b20S1.90 Manganese carbonate MnC:O55,18 And phosphor 3Ca, ( POa )2 Ca(F, (
J) Form 2/SA, Mn.

Comparing the results obtained with the conventional device shown in Figure 1 and the device of the present invention, it was found that (xwaAg) was the best result for the phosphor. In comparison, as shown in the figure, the phosphor of the present invention is smaller than the phosphor of the conventional device.
) was confirmed to be high brightness and stable.

In the above embodiment, the firing container (8) filled with the synthetic material is moved by the transfer body (6), but the container (8) is moved by a button without using the transfer body (16). You can also use 171 to move by pushing directly (・.

Although the present invention is limited to the production of halophosphate phosphors, it can also be widely used in the production of other activated phosphors.

〔Effect of the invention〕

According to the present invention, by injecting inert gas from near the outlet of the furnace body in the opposite direction to the direction of movement of the fired body, the pressure in the cooling zone is increased and the cracked gas generated in the preheating zone is reliably discharged. The antimony chloride gas required for phosphor production generated in the firing zone can be retained.

Furthermore, by blocking air from outside the furnace body with an inert gas, the generation of phosphor and the oxidation of the activator can be prevented, and the efficiency of emitting C of the phosphor can be increased.

Furthermore, by increasing the retention of gas within the furnace body, it is possible to increase heat utilization efficiency, achieve a significant energy saving effect, and reduce manufacturing costs.

[Brief explanation of the drawing]

】・Figure 1 (0) (Force is an explanatory diagram of the conventional device and its firing temperature - firing time relationship diagram, Figure 2 (α) (Force is a detailed explanatory diagram of the present invention and its firing temperature – firing time Figure 5 is a comparison diagram of the relative brightness of firefly C bodies. (1) Furnace body, (2) Inlet part, (3) Outlet part, (8)... Container, (IIJ...Inert gas introduction device.

Claims (1)

[Claims] (1) Firing is carried out while moving the phosphor synthetic material filled in a fire-resistant firing container formed into a hollow and long shape from the entrance to the exit. and an inert gas introduction device that is provided at the outlet of the furnace body and introduces an inert gas into the vicinity of the outlet of the furnace body in a direction opposite to the moving direction of the phosphor synthetic material. Manufacturing equipment for phosphor R6