CN111302617B - Tail gas recycling system for preparing optical fiber preform by gas phase method - Google Patents
Tail gas recycling system for preparing optical fiber preform by gas phase method Download PDFInfo
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- CN111302617B CN111302617B CN202010345401.6A CN202010345401A CN111302617B CN 111302617 B CN111302617 B CN 111302617B CN 202010345401 A CN202010345401 A CN 202010345401A CN 111302617 B CN111302617 B CN 111302617B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D50/00—Combinations of methods or devices for separating particles from gases or vapours
- B01D50/20—Combinations of devices covered by groups B01D45/00 and B01D46/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/0144—Means for after-treatment or catching of worked reactant gases
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01846—Means for after-treatment or catching of worked reactant gases
Abstract
The invention provides a tail gas recycling system for preparing an optical fiber preform by a vapor phase method. The system comprises a pump end gas transmission sealing device, a dust waste heat collecting device, a filter screen, a dehydration and dust removal device, a gas filter, a vacuum generator, a gas storage tank, a gas separation device, a Cl2 storage tank, an O2/He storage tank, a filtering and pressure regulating device, a gas cache tank, a detector, a flowmeter and a corresponding pipeline. The system not only can utilize the waste heat in the production process, but also can separate dust (mainly high-purity silicon dioxide can be used for glass preparation) and tail gas. The tail gas can be further separated into O2/He mixed gas and Cl2 for process production. The system is a sealed circulating system, can comprehensively utilize dust, tail gas and waste heat after reaction, and also avoids the problems of resource waste, high waste gas and waste water treatment cost and possible environmental pollution caused by treating reaction products as wastes.
Description
Technical Field
The invention belongs to the technical field of optical fiber perform preparation, and particularly relates to a tail gas recycling system for preparing an optical fiber perform by a gas phase method.
Background
With the development of science and technology, the application of optical fiber materials in the fields of communication, industrial processing, military, medical treatment, aerospace and the like has achieved great success. Silica fibers are among the most widely used. The optical fiber prefabricated rod is used as the base material of optical fiber and contains high purity silica and co-doped agent. The existing method for preparing the optical fiber preform is a vapor deposition method, and mainly comprises four preparation methods of MCVD, PCVD, OVD and VAD. The deposition principle is that process gases such as high-purity O2, high-purity He, high-purity SiCl4, high-purity GeCl4, high-purity POCl3 and high-purity Cl2 (the purity is 99.999%) are conveyed to a deposition area to carry out chemical reaction under the heating condition to generate substances such as high-purity SiO2, GeO2 and P2O 5. The He has high thermal conductivity and is used for deposition, so that the temperature distribution in the lining pipe is uniform, and the quality of the optical fiber perform rod is improved; o2 is used as a reaction gas and is usually in excess of the reaction gas in order to sufficiently carry out the reaction and maintain a suitable pressure in the tube. Therefore, a great deal of dust, tail gas and heat exist at the tail end of the reaction, wherein the dust is mainly composed of particles such as SiO2, GeO2, P2O5 and the like, and the tail gas is mainly O2, He, Cl2 and a small amount of H2O. The chemical reaction equation of the deposition in the tube is as follows:
SiCl4+ O2= SiO2+ Cl2
GeCl4+ O2= GeO2+ Cl2
4POCl3+ 3O2= 2P2O5+ 6Cl2
because the dust particles are extremely small and the tail gas is a strong acid gas, if the tail gas directly enters the air, the environment is greatly polluted. The main treatment methods at present are: and sending the dust and the tail gas at the tail end of the preparation equipment into a spray tower for dedusting and acid-base neutralization reaction by utilizing strong air draft, then discharging clean gas into the air, and carrying out next treatment on the wastewater. In addition, the temperature of the tail gas which is just reacted is extremely high, reaching 500-1000 ℃, and the tail gas is not normally treated and naturally cooled in the air in the method. The method has the advantages of high energy consumption, resource waste, high O2, He and Cl2 content in the tail gas and high purity, and can save a lot of energy and resources if reasonably utilized, particularly the He resource is extremely deficient, and the cost is quite expensive.
There are also some He recovery techniques that involve subjecting the spray tower treated clean gas (mainly O2, He, and a certain amount of moisture, chloride and dust) to a series of complex treatments followed by separation and purification of the He. Although He can be recycled, the method still needs a large amount of energy, has complex process and wastes heat, O2, Cl2 and other resources.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a tail gas recycling device for preparing an optical fiber perform rod by a gas phase method, which comprises a pump end gas transmission device, a dust waste heat collecting device, a filter screen, a dehydration and dust removal device, a first gas filter, a vacuum generator, a gas cache tank, a gas separation device, a Cl2 storage tank, an O2/He storage tank, a first filtering and pressure regulating device, a second filtering and pressure regulating device, a gas storage tank, a detector, a flowmeter, a second gas filter and corresponding pipelines, wherein the pump end gas transmission device comprises a gas cabinet gas supply device, a gas end chuck and a sealing device of a vapor deposition device, a liner pipe and a pump of the vapor deposition device which are sequentially connectedThe outlet of the pump end gas transmission device is connected with the dust waste heat collecting device, the filter screen, the dehydration and dust removal device, the first gas filter, the vacuum generator, the gas cache tank and the gas separation device are sequentially connected, and the first output port of the gas separation device is sequentially connected with the O2The first output port of the gas separation device is connected with the Cl2 storage tank and the second filtering and pressure regulating device and then connected with the gas storage tank. All devices of the system form a circulating system, so that the tail gas can be recycled, and the pollution to the atmosphere can be avoided.
According to one aspect of the invention, the apparatus and use of the system are as follows:
the pump end gas transmission sealing device comprises a pipeline and a sealing device. The pipeline is used for connecting a subsequent dust collecting device at the tail end of the liner pipe, and the sealing device is used for sealing the joint. The pipeline is made of heat-resistant and corrosion-resistant non-metallic materials, preferably high-purity silica glass or Teflon materials; the sealing means in contact with the exhaust gases are also made of a heat-resistant and corrosion-resistant material, preferably of a fluoroelastomer.
The dust waste heat collecting device is cylindrical and similar to a vacuum flask in structure, the inner layer is made of high-purity silica glass with the thickness of 0.5-1mm, the outer layer is made of metal and nonmetal materials (covered with a heat-insulating layer), and water is filled between the inner layer and the outer layer. The heat in the tail gas is absorbed by the water, which is beneficial to the deposition of the dust in the collecting device. And the hot water can be used for bathing in a factory building.
The filter screen is composed of filter screens with the specifications of 10 mu m, 5 mu m, 2 mu m and 0.5 mu m in sequence and is used for filtering gas discharged from the dust collecting device.
The dehydration and dust removal device has the function of dehydrating the gas (containing a small amount of moisture) coming from the filter screen and further removing dust by using the filter screen with the diameter of 0.05 mu m.
The connection of the devices adopts a high-purity Teflon pipeline, and a VCR joint is preferably selected as a connector.
The gas filter has the filtration specification of 0.02 mu m and is used for filtering gas.
The vacuum generator is used for extracting tail gas passing through the filter screen and sending the tail gas into the gas storage tank, so that the pressure in the lining pipe is stable. The blade part of the vacuum pump is made of high-purity Teflon material.
The gas storage tank is used for storing O2, He and Cl2 gases (the purity is 99.9%) pumped by a vacuum pump, the storage tank is made of stainless steel 316L, and the pressure-resistant grade of the storage tank is 7 MPa.
The gas separation device can be made of stainless steel 316L and is used for separating O2, He and Cl 2. The separation method is based on the characteristic that Cl2 is easy to liquefy at high pressure (600-700 kPa) or-34 ℃ and O2/He is extremely difficult to liquefy.
The Cl2 storage tank is used for storing separated Cl2, and the tank body can be made of stainless steel 316L.
The O2/He storage tank is used for storing separated O2/He, and the tank body can be made of stainless steel 316L.
The filtering pressure regulating device is used for filtering gas in an O2/He storage tank (a 0.003 mu m gas filter), regulating the gas to a certain pressure through a pressure regulating valve and conveying the gas to a gas buffer tank.
The detector is used for detecting the concentration of O2 and He in O2/He mixed gas (the content of O2/He in the mixed gas reaches 99.9 percent, and the residual 0.1 percent is mainly Cl 2) flowing through the detector.
The flowmeter is used for metering the O2/He gas flow rate flowing to the gas phase deposition gas end.
According to another aspect of the present invention, the exhaust gas recycling system provided by the present invention has practical value based on the following principle:
(1) the purity requirements of raw materials such as high-purity O2, high-purity He, high-purity SiCl4, high-purity GeCl4, high-purity POCl3 and high-purity Cl2 in vapor deposition are all 99.999 percent. It is understood that the requirement of purity means that the contents of metal ions and OH are respectively below 1ppm, and the loss of the optical fiber is greatly influenced by the metal ions and OH. The whole process of the vapor deposition is a sealed system, all substances in the tail gas are reactants or products, and the substances are not harmful to the chemical vapor deposition, so that a theoretical basis is provided for recycling the tail gas.
(2) The purity of the mixed gas of O2, He and Cl2 in the tail gas can reach more than 99.9 percent, and the gas can be further separated into O2/He mixed gas (the purity is more than 99.9 percent) and Cl2 (the purity is more than 99.9 percent) through the liquefaction of Cl 2. In which O2 is used as the excess reaction gas and He is used as the heat transfer gas, the flow rate accuracy in vapor deposition does not need to be particularly high (5 slm for O2 deposition, which may fluctuate by 50 sccm; 1slm for He deposition, which may fluctuate by 10 sccm). While the purity of the O2/He mixed gas was 99.9%, if the O2/He concentration ratio detected by the detector was 2:1, when 3slm of this mixed gas was used, the O2 flow rate was 2slm (the remaining 3slm gas supply tank), the He flow rate was 1slm, and the flow error thereof was 3 sccm. Completely meets the process requirements.
(3) Cl2 is mainly used for dehydration treatment during optical fiber deposition (such as solution method for preparing rare earth doped optical fiber), and the stored Cl2 also completely meets the requirements of the process. The excess Cl2 can be used in other industrial processes.
The tail gas recycling system for preparing the optical fiber preform by the gas phase method provided by the invention not only can utilize the waste heat in the production process, but also can separate dust (mainly high-purity silicon dioxide can be used for preparing glass) and tail gas. The tail gas can be further separated into O2/He mixed gas and Cl2 for process production. The system is a sealed circulating system, can comprehensively utilize dust, tail gas and waste heat after reaction, and also avoids the problems of resource waste, high waste gas and waste water treatment cost and possible environmental pollution caused by treating reaction products as wastes.
Drawings
In the figure, 1 is a gas end chuck and a sealing device of vapor deposition equipment, 2 is a liner tube, 3 is a pump end chuck and a sealing device of vapor deposition equipment, 4 is a high-purity quartz tube, 5 is a dust waste heat collecting device, 6 is a high-purity Teflon tube, 7 is a pipeline (316 l EP polishing, the dotted line shows that the process is the same as O2/He when in use) recycled by Cl2, and 8 is an O2/He access pipeline (316 l EP polishing). The devices or devices such as the other filter screens, the dehydration and dust removal device, the gas filter, the vacuum generator, the gas storage tank, the gas separation device, the Cl2 storage tank, the O2/He storage tank, the filtration and pressure regulation device, the gas buffer tank, the detector, the flowmeter and the like are shown in the figure. It should be noted that all vessels or pipes utilizing stainless steel 316L are EP grade. The piping shown in the remaining figures is stainless steel 316L EP grade piping, except that the piping labeled 6 is high purity teflon piping.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention takes MCVD to prepare passive matching optical fiber prefabricated rod for optical fiber laser as an example for explanation.
Firstly, gas is supplied into a gas cabinet as O2, He, SiCl4 and GeCl4 (the flow rates are respectively 5slm, 2slm, 200sccm and 40 sccm), the gas enters a liner tube through a gas end, a chemical reaction is carried out under the action of oxyhydrogen flame, and products are SiO2, GeO2, Cl2, SiO2 and GeO2 particles which are a considerable part are deposited on the wall of the liner tube under the thermophoresis principle. The tail gas entering the pump end mainly comprises O2, He, SiO2, GeO2 and Cl 2.
When tail gas enters the dust waste heat collecting device, dust is deposited, and simultaneously, waste heat is used for heating tap water for bathing. The residual gas is filtered by a filter screen, and the dust content is below 0.01 percent. At the moment, residual moisture in the gas is removed by a dehydration and dust removal device, and the dust content is further reduced to 0.001 percent.
The impeller part of the vacuum pump of the vacuum generator is made of Teflon and used for pumping the tail gas at the MCVD pump end outwards and storing the tail gas in the gas storage tank, so that the pressure in the lining pipe is stable. Which is the power plant of the whole circulation system.
The separation apparatus, in this example using a-40 ℃ cold bath (i.e. the separation tank is placed in a-40 ℃ thermostated environment), will liquefy Cl2 while O2, He is still in a gaseous state. By pumping liquefied Cl2 to a Cl2 storage tank and repeating this step several times, the purity of the mixture of O2 and He can be increased to 99.9%. The O2/He mixer was then pumped into the O2/He storage tank for future use.
The filtering pressure regulating device, the gas buffer tank, the detector, the flowmeter and the gas filter are used for regulating the O2/He storage tank to a certain pressure, and the O2/He storage tank enters the gas end for recycling after concentration measurement, flow control and gas filtration. If the flow rate is 3slm and the O2/He concentration ratio is 2:1, the O2 flow rate and the He flow rate for recycling are 2slm and 1slm, respectively. The gases supplied to the gas holder to ensure the reaction proceeded normally were O2, He, SiCl4, and GeCl4 (flow rates 3slm, 1slm, 200sccm, and 40sccm, respectively). It should be noted that all of the equipment and piping here need to be at the same temperature as the gas cabinet process gas.
The tail gas of the preform prepared by the gas phase method can be recycled by the circulating system.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The tail gas recycling device for preparing the optical fiber perform rod by the vapor phase method is characterized by comprising a pump end gas transmission device, a dust waste heat collecting device, a filter screen, a dehydration and dust removal device, a first gas filter, a vacuum generator, a gas cache tank, a gas separation device and Cl2Storage tank, O2The He storage tank, the first filtering and pressure regulating device, the second filtering and pressure regulating device, the gas storage tank, the detector, the flowmeter, the second gas filter and the corresponding pipeline, wherein the pump end gas transmission device comprises a gas holder gas supply device, a gas end chuck and a sealing device of vapor deposition equipment, a liner pipe and a pump end chuck of the vapor deposition equipment which are sequentially connectedThe sealing device, the exit linkage of pump end gas transmission device dust waste heat collection device, filter screen, dehydration dust collector, first gas filter, vacuum generator, gaseous buffer tank, gas separation device connect gradually, and O is connected gradually to gas separation device's first delivery outlet2The first output port of the gas separation device is connected with Cl2The storage tank and the second filtering and pressure regulating device are connected with the gas storage tank;
the dust waste heat collecting device is cylindrical and has a structure similar to a vacuum flask, the inner layer is made of high-purity silica glass with the thickness of 0.5-1mm, the outer layer is a heat insulation layer covered by a metal or non-metal material, water is arranged between the inner layer and the heat insulation layer, and the dust waste heat collecting device can enable dust to be deposited in the collecting device by absorbing heat in tail gas through the water;
the gas separation device is used for separating O2He and Cl2Separating with stainless steel 316L material, wherein the separation method is based on Cl2Is easy to liquefy at high pressure of 600 ℃ and 700kPa or-34 ℃ and O2the/He is extremely difficult to liquefy.
2. The apparatus of claim 1, wherein the filter screen comprises filter screens of 10 μm, 5 μm, 2 μm, and 0.5 μm in sequence.
3. The apparatus of claim 1, wherein the dehydration dust removing apparatus is configured to dehydrate the filtered gas and the remaining small amount of water, and further remove dust with a 0.05 μm filter screen.
4. The apparatus of claim 1, wherein the conduit is a Teflon conduit and the interface is a VCR connector.
5. The apparatus of claim 1, wherein the first and second gas filters have a filter size of 0.02 μm.
6. The apparatus of claim 1, wherein the gas buffer tank is used for storing O pumped by the vacuum pump2、He、Cl2And the gas buffer tank is made of a stainless steel 316L material, and the pressure resistance grade of the gas buffer tank is 7 MPa.
7. The apparatus of claim 1, wherein the Cl is the gas in the apparatus for recycling exhaust from the optical fiber preform manufacturing process2Storage tanks for storing separated Cl2The tank body is made of stainless steel 316L, and O2Storage tank for/He for storing separated O2and/He, the tank body is made of stainless steel 316L.
8. The apparatus of claim 1, wherein the first filtering and pressure-regulating means is a device for recycling exhaust gas from a vapor-phase process for manufacturing an optical fiber preform2The gas in the/He storage tank passes through a 0.003 mu m gas filter, is regulated to a certain pressure by a pressure regulating valve and is conveyed to a gas storage tank.
9. The apparatus of claim 1, wherein the detector is configured to detect O flowing through the detector2O in mixed gas of/He2He, said flowmeter is used for metering O flowing to the gas-phase deposition gas end2The volume flow rate of the/He gas.
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| AU7185900A (en) * | 2000-01-14 | 2001-07-19 | Boc Group, Inc., The | Helium recovery process |
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| CN1176941A (en) * | 1996-07-26 | 1998-03-25 | 普拉塞尔技术有限公司 | Helium recovery for optical fiber mfg. |
| CN1576249A (en) * | 2003-07-17 | 2005-02-09 | 波克股份有限公司 | Method for the recovery and recycle of helium and chlorine |
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