CN212356559U

CN212356559U - Quartz sand high-temperature chlorination reaction system

Info

Publication number: CN212356559U
Application number: CN202020808179.4U
Authority: CN
Inventors: 田辉明; 田正芳; 黄林勇; 江军民; 陈中文
Original assignee: Huanggang Normal University
Current assignee: Huanggang Normal University
Priority date: 2020-05-15
Filing date: 2020-05-15
Publication date: 2021-01-15
Anticipated expiration: 2030-05-15

Abstract

The utility model relates to a quartz sand high-temperature chlorination reaction system, which comprises a chlorination tank, wherein the chlorination tank is connected with a quartz feeding device, a chlorine recovery device and a quartz collecting device; the chlorination tank comprises a graphite inner container and a ceramic protective layer covering the outer surface of the graphite inner container, and the bottom of the chlorination tank is a cone; the chlorine feeding device comprises a plurality of graphite pipes, and the graphite pipes are inserted into the bottom of the chlorination tank from the top. The chlorination tank body of the utility model is composed of the graphite inner container and the ceramic protective layer, and can perform chlorination operation at 1500 ℃ for a long time, and simultaneously avoid high-temperature oxidation of the tank body; the chlorine is conveyed through the graphite pipes which are directly communicated with the bottom of the chlorination tank, so that the gas-solid resistance between the heated chlorine and sand particles can be reduced, and the uniformity of chlorination of materials is ensured; the bottom of the chlorination tank is conical, so that the material is convenient to discharge.

Description

Quartz sand high-temperature chlorination reaction system

Technical Field

The utility model relates to a quartz sand high temperature chlorination system belongs to non-metallic mineral deep-processing technical field.

Background

High-purity quartz sand for photovoltaic and electronic products used in China are mostly imported from the company of Ennimine in the United states. The yield of various high-purity quartz sand products produced by the company per year is more than 3 million tons, most manufacturers of the high-purity quartz sand for domestic photovoltaic and electronic products in China adopt domestic igneous vein quartz or imported igneous vein quartz as raw materials to produce the high-purity quartz sand for the electronic products, and although some technical indexes of the produced products reach or exceed the products of the Unimine company in America, the quality of the products is unstable and the products cannot be industrially produced in large batch. Apart from the influence of raw material ores, the main reason is that the key impurity removal equipment in the production process and the production process is not advanced, especially the high-temperature chlorination equipment after chemical purification. The domestic high-temperature chlorination equipment is prepared by quartz glass tubes, but the China can not produce the quartz glass tubes with large calibers (the diameter is more than 500 mm) so far; the prohibition of the large-diameter quartz glass tube against China is applied to China, so that the existing high-purity quartz sand high-temperature chlorination equipment cannot be produced in large scale in China. In addition, since high purity silica glass is crystallized at 1250 ℃ or more, it can be operated only for a long period of time at a temperature of about 1100 ℃. In order to reduce the impurities in the chemically purified quartz sand to the limit, chlorination impurity removal needs to be carried out on the quartz sand at the high temperature of over 1450 ℃, so that the 13 metal impurities in the quartz sand can be reduced to the limit. And the chlorination tank made of high-purity quartz glass cannot meet the requirements of process conditions. In the patent CN102432022B applied before, the high-temperature chlorination device is made of high-purity quartz glass, the bottom of the chlorination tank is provided with a support column, a microporous plate is arranged on the column, added chlorine enters the kettle from the side between the microporous plate and the bottom of the kettle and performs chlorination reaction with heated high-temperature quartz sand, and chlorine salt gas generated after the reaction enters the cooling tank from a degassing pipe at the top of the kettle to be cooled. This device also has some drawbacks: 1, the use temperature is low and can only be used between 1100 ℃ and 1250 ℃; 2, a dead angle is formed at the bottom of the container, so that chlorinated materials are easy to accumulate; 3, certain pressure will be born between during operation micropore board and the cauldron bottom, and after pressure reached certain degree, quartz glass probably can break, has the potential safety hazard. The high-temperature chlorination reaction kettle made of platinum-rhodium alloy can meet the requirements, but the manufacturing cost is too high, and industrialization is difficult to realize. High purity silicon carbide materials can withstand high temperatures of 1500 ℃, but at these temperatures silicon tetrachloride and carbon are formed by reaction with chlorine gas. Therefore, after long-time research, a new high-temperature chlorination system for high-purity quartz sand is developed, and the method successfully solves the problem of the method for removing impurities in quartz sand powder to the limit, so that the purification process technology of the high-purity quartz sand in China is led to advance to the world advanced line. The relevant literature data is consulted, and no relevant literature data or academic reports are found.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to provide a quartz sand high temperature chlorination system, the high temperature chlorination reation kettle in this system can work for a long time under high temperature, makes the impurity element in the quartz sand reach minimum.

The utility model provides a scheme that above-mentioned technical problem adopted is:

a quartz sand high-temperature chlorination reaction system comprises a chlorination tank, wherein the chlorination tank is connected with a quartz feeding device, a chlorine recovery device and a quartz collecting device; the chlorination tank comprises a graphite inner container and a ceramic protective layer covering the outer surface of the graphite inner container, and the bottom of the chlorination tank is a cone; the chlorine feeding device comprises a plurality of graphite pipes, and the graphite pipes are inserted into the bottom of the chlorination tank from the top.

Preferably, the quartz feeding device comprises a quartz sand preheating tank, and the top of the quartz sand preheating tank is connected with a quartz sand bin, a protective gas feeding pipe, a thermometer and an exhaust pipe; the lower end pipe orifice of the protective gas feeding pipe extends to the bottom of the quartz sand preheating tank; valves are connected among the quartz sand bin, the protective gas feeding pipe, the exhaust pipe and the quartz sand preheating tank; and a discharge port at the bottom of the quartz sand preheating tank is connected with the top of the chlorination tank through a valve and a pipeline.

Preferably, the chlorine feeding device comprises a chlorine tank, a reduced pressure gasification tank and a graphite pipe which are sequentially connected through pipelines, a valve and a flowmeter are connected between the reduced pressure gasification tank and the graphite pipe, and the chlorine tank is arranged on the electronic scale.

Preferably, the chlorine recovery unit comprises a gas cooling kettle, a water absorption tank and an induced draft fan which are sequentially connected with a pipeline at the top of the chlorination tank.

Preferably, the quartz collecting device comprises a material cooling kettle connected with a discharge port at the bottom of the chlorination tank, and a cyclone dust collector, a bag-type dust collector and an induced draft fan which are sequentially connected with pipelines of the material cooling kettle; and a water cooling sleeve is arranged on the outer wall of the pipeline between the material cooling kettle and the discharge port at the bottom of the chlorination tank.

Preferably, the chlorine gas feeding device is connected with the chlorine gas recovery device through a chlorine gas pump.

Preferably, the top of the chlorination tank is also connected with a high-temperature thermometer.

Preferably, the chlorination tank is heated externally by a high temperature furnace, or by microwave or plasma heating.

Compared with the prior art, the utility model discloses following beneficial effect has:

the chlorination tank body is composed of the graphite inner container and the ceramic protective layer, chlorination can be carried out at 1500 ℃ for a long time, and high-temperature oxidation of the tank body is avoided; the chlorine is conveyed through the graphite pipes which are directly communicated with the bottom of the chlorination tank, so that the gas-solid resistance between the heated chlorine and sand particles can be reduced, and the uniformity of chlorination of materials is ensured; the bottom of the chlorination tank is conical, so that the material is convenient to discharge.

Drawings

FIG. 1 is a schematic structural diagram of a quartz sand high-temperature chlorination reaction system of the present invention.

The figures in the drawings are labeled as:

1, a chlorination tank; 2, a graphite inner container; 3, a ceramic protective layer; 4, a graphite tube; 5, a thermometer; 6, preheating a quartz sand tank; 7, a quartz sand bin; 8, a protective gas feeding pipe; 9, an exhaust pipe; 10, chlorine gas tanks; 11, a reduced-pressure gasification tank; 12, a flow meter; 13, an electronic scale; 14, cooling the kettle by gas; 15, a water absorption tank; 16, a draught fan; 17, cooling the material in a kettle; 18, a cyclone dust collector; 19, a bag-type dust collector; 20, water cooling jacket; 21, chlorine pump.

Detailed Description

For better understanding of the present invention, the following examples are further illustrative of the present invention, but the present invention is not limited to the following examples.

Example 1

As shown in fig. 1, a quartz sand high-temperature chlorination reaction system comprises a chlorination tank 1, wherein the chlorination tank 1 is connected with a quartz feeding device, a chlorine recovery device and a quartz collecting device; the chlorination tank 1 adopts the graphite inner container 2, the high-purity graphite material product (4N or more) does not reduce the strength at high temperature and does not react with chlorine, and silicon carbide ceramic or silicon nitride ceramic or composite ceramic of silicon carbide and silicon nitride and other ultrahigh-temperature ceramic are adopted as the ceramic protective layer 3 on the outer wall of the chlorination tank 1 in consideration of the fact that graphite is easily oxidized when being contacted with oxygen in the air at high temperature. The bottom of the chlorination tank 1 is a cone, so that the material is conveniently discharged; chlorine feed arrangement includes many graphite pipes 4, and many graphite pipes 4 can be as being responsible for and the auxiliary pipe collocation use, according to graphite pipe 4's position, with graphite pipe 4 direct insert tank bottoms or inner wall department from chlorination tank 1's top, reduce the gas-solid resistance between chlorine heating and the sand granule and guarantee the homogeneity of material chlorination. The top of the chlorination tank 1 is also connected with a high-temperature thermometer 5, and the part of the thermometer 5 extending into the tank body is protected by a high-temperature sleeve. The chlorination tank 1 adopts an external heating mode, and the heat source adopts a high-temperature furnace adopting an electric heating mode, such as a resistance furnace, a medium-frequency smelting furnace, a silicon-molybdenum rod electric furnace, a silicon-carbon rod electric furnace, a graphite rod electric furnace and a graphene electric furnace, and can also adopt heat sources adopting other modes of microwave, plasma and the like.

The quartz feeding device comprises a quartz sand preheating tank 6, and the top of the quartz sand preheating tank 6 is connected with a quartz sand bin 7, a protective gas feeding pipe 8, a thermometer 5 and an exhaust pipe 9; the lower end pipe orifice of the protective gas feeding pipe 8 extends to the bottom of the quartz sand preheating tank 6; valves are connected among the quartz sand bin 7, the protective gas feeding pipe 8, the exhaust pipe 9 and the quartz sand preheating tank 6; and a discharge port at the bottom of the quartz sand preheating tank 6 is connected with the top of the chlorination tank 1 through a valve and a pipeline.

Chlorine feed arrangement is including chlorine gas jar 10, decompression gasification jar 11 and graphite pipe 4 of pipe connection in proper order, all be connected with valve and flowmeter 12 between decompression gasification jar 11 and the graphite pipe 4. In order to control the amount of chlorine, the chlorine tank 10 may be placed on an electronic scale 13, and the chlorination tank 1 may be provided with a weight detecting instrument.

The chlorine gas recovery device comprises a gas cooling kettle 14, a water absorption tank 15 and a draught fan 16 which are sequentially connected with a pipeline at the top of the chlorination tank 1.

The quartz collecting device comprises a material cooling kettle 17 connected with a discharge hole at the bottom of the chlorination tank 1, and a cyclone dust collector 18, a bag-type dust collector 19 and an induced draft fan 16 which are sequentially connected with the material cooling kettle 17 through pipelines; and a water cooling jacket 20 is arranged on the outer wall of the pipeline between the material cooling kettle 17 and the discharge port at the bottom of the chlorination tank 1.

The chlorine feeding device is connected with the chlorine recovery device through a chlorine pump 21, specifically, the reduced-pressure gasification tank 11 can be connected with a pipeline between the gas cooling kettle 14 and the water absorption tank 15, and for saving high-purity chlorine resources, for intermittent high-temperature chlorination, chlorine cooled to room temperature by the gas cooling kettle 14 can be sent to the reduced-pressure gasification tank 11 through the chlorine pump 21 to be used in a closed cycle mode. For continuous high-temperature chlorination, cooled chlorine gas can be compressed and liquefied again and then is filled into a chlorine gas tank 10 for workshop use.

The corresponding positions of the inlet, the outlet and the conveying pipeline of the corresponding parts in the quartz sand high-temperature chlorination reaction system can be provided with valves as required.

While the foregoing is directed to the preferred embodiment of the present invention, it will be understood that the invention is not limited thereto, and that various modifications and changes can be made by those skilled in the art without departing from the principles of the invention.

Claims

1. The quartz sand high-temperature chlorination reaction system is characterized by comprising a chlorination tank, wherein the chlorination tank is connected with a quartz feeding device, a chlorine recovery device and a quartz collecting device; the chlorination tank comprises a graphite inner container and a ceramic protective layer covering the outer surface of the graphite inner container, and the bottom of the chlorination tank is a cone; the chlorine feeding device comprises a plurality of graphite pipes, and the graphite pipes are inserted into the bottom of the chlorination tank from the top.

2. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein the quartz feeding device comprises a quartz sand preheating tank, and a quartz sand silo, a protective gas feeding pipe, a thermometer and an exhaust pipe are connected to the top of the quartz sand preheating tank; the lower end pipe orifice of the protective gas feeding pipe extends to the bottom of the quartz sand preheating tank; valves are connected among the quartz sand bin, the protective gas feeding pipe, the exhaust pipe and the quartz sand preheating tank; and a discharge port at the bottom of the quartz sand preheating tank is connected with the top of the chlorination tank through a valve and a pipeline.

3. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein the chlorine gas feeding device comprises a chlorine gas tank, a reduced pressure gasification tank and a graphite pipe which are sequentially connected through pipelines, a valve and a flowmeter are connected between the reduced pressure gasification tank and the graphite pipe, and the chlorine gas tank is arranged on an electronic scale.

4. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein the chlorine gas recovery device comprises a gas cooling kettle, a water absorption tank and an induced draft fan which are sequentially connected with a top pipeline of the chlorination tank.

5. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein the quartz collecting device comprises a material cooling kettle connected with a discharge port at the bottom of the chlorination tank, and a cyclone dust collector, a bag-type dust collector and an induced draft fan which are sequentially connected with pipelines of the material cooling kettle; and a water cooling sleeve is arranged on the outer wall of the pipeline between the material cooling kettle and the discharge port at the bottom of the chlorination tank.

6. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein the chlorine gas feeding device is connected with the chlorine gas recovery device through a chlorine gas pump.

7. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein a high-temperature thermometer is further connected to the top of the chlorination tank.

8. The quartz sand high-temperature chlorination reaction system according to claim 1, wherein the chlorination tank is heated externally by a high-temperature furnace, or by a microwave oven or a plasma oven.