CN117550786A - Bulk mixing unit, gaseous raw material feeding device and feeding method - Google Patents
Bulk mixing unit, gaseous raw material feeding device and feeding method Download PDFInfo
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- CN117550786A CN117550786A CN202311479727.8A CN202311479727A CN117550786A CN 117550786 A CN117550786 A CN 117550786A CN 202311479727 A CN202311479727 A CN 202311479727A CN 117550786 A CN117550786 A CN 117550786A
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- 239000002994 raw material Substances 0.000 title claims abstract description 220
- 238000002156 mixing Methods 0.000 title claims abstract description 92
- 238000000034 method Methods 0.000 title claims abstract description 29
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 103
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 103
- 239000010936 titanium Substances 0.000 claims abstract description 103
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 99
- 239000010703 silicon Substances 0.000 claims abstract description 99
- 239000000463 material Substances 0.000 claims abstract description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000009833 condensation Methods 0.000 claims abstract description 23
- 230000005494 condensation Effects 0.000 claims abstract description 23
- 239000007789 gas Substances 0.000 claims description 119
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 98
- 238000001704 evaporation Methods 0.000 claims description 34
- 230000008020 evaporation Effects 0.000 claims description 31
- 238000005485 electric heating Methods 0.000 claims description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 229910003902 SiCl 4 Inorganic materials 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000012159 carrier gas Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 18
- 239000002245 particle Substances 0.000 abstract description 11
- 238000000151 deposition Methods 0.000 abstract description 9
- 230000008021 deposition Effects 0.000 abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 9
- 239000000377 silicon dioxide Substances 0.000 abstract description 9
- 239000004408 titanium dioxide Substances 0.000 abstract description 9
- 230000003287 optical effect Effects 0.000 abstract description 6
- 238000007740 vapor deposition Methods 0.000 abstract description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 30
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 19
- 239000005049 silicon tetrachloride Substances 0.000 description 19
- 239000000203 mixture Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000010425 asbestos Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 229910052895 riebeckite Inorganic materials 0.000 description 3
- NRTJGTSOTDBPDE-UHFFFAOYSA-N [dimethyl(methylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[SiH2]O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C NRTJGTSOTDBPDE-UHFFFAOYSA-N 0.000 description 2
- 230000004323 axial length Effects 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005008 domestic process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B1/00—Preparing the batches
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The invention provides a bulk mixing unit, a gaseous raw material feeding device and a feeding method, which are used for preparing quartz glass by a vapor deposition method. The body-increasing mixing unit comprises a first material conveying pipeline, a second material conveying pipeline, a tank body, a mixing output pipeline and a compensating gas input pipeline. The gaseous raw material feeding device comprises an integral mixing unit. The gaseous raw material feeding method is implemented on a gaseous raw material feeding device. By using the bulk mixing unit, the gaseous raw material feeding device and the feeding method, the gaseous raw material containing silicon and the gaseous raw material containing titanium can be uniformly premixed in advance in the tank according to a certain mass ratio, condensation and dew do not occur, the mass fraction of each component in the mixed particles of silicon dioxide and titanium dioxide deposited on the deposition surface can be ensured to be fixed, the components are uniform, the deposition rate is stable, and the titanium doped quartz glass with higher optical uniformity and zero expansion can be prepared.
Description
Technical Field
The invention relates to the technical field of quartz glass preparation, in particular to a bulk mixing unit, a gaseous raw material feeding device and a gaseous raw material feeding method.
Background
Titanium doped silica glass is an excellent optical material because of its extremely low coefficient of thermal expansion (about 5.7x10 -7 High thermal processability, and plays an important role in the high-tech fields such as astronomy and semiconductors.
Currently, domestic processes for producing titanium doped quartz glass include axial vapor deposition (VAD) or Chemical Vapor Deposition (CVD). For example, patent document 1 discloses a method of producing silicon tetrachloride (SiCl) as a silicon-containing chemical liquid material having a purity of > 99.99% 4 At > 85 ℃ and titanium-containing chemical liquid raw material titanium tetrachloride (TiCl) 4 At > 135 ℃ or by gasifying Octamethyltetrasiloxane (OMCTS) which is a high purity silicon-containing chemical liquid raw material and titanium tetrachloride (TiCl) which is a titanium-containing chemical liquid raw material at > 180 DEG c 4 At > 135 ℃); introducing gasified silicon tetrachloride or octamethyltetrasiloxane raw material and titanium tetrachloride raw material into hydrogen-oxygen flame respectively, controlling the temperature of a deposition surface to 900-950 ℃, and generating mixed powder particles of silicon dioxide and titanium dioxide through chemical vapor deposition reaction, wherein the particle size is not more than 1 mu m.
The condensation and dewing phenomena can exist in the gaseous silicon-containing raw materials and the gaseous titanium-containing raw materials in the transmission process, so that equipment and pipelines are polluted and blocked quickly, the gaseous silicon-containing raw materials and the gaseous titanium-containing raw materials are difficult to hydrolyze in hydrogen-oxygen flame generated by a burner in a fixed mass ratio, and the mass ratio and total amount of generated silicon dioxide particles and titanium dioxide particles are unstable; meanwhile, the random movement time of the gaseous silicon-containing raw materials and the gaseous titanium-containing raw materials before hydrolysis in hydrogen-oxygen flame generated by a burner is extremely short, and a uniform mixing state is difficult to achieve, so that generated silicon dioxide particles and titanium dioxide particles cannot be uniformly mixed; in both cases, no titanium-doped silica glass with zero expansion could be produced and the optical uniformity was lowered.
Disclosure of Invention
The invention aims to provide a bulk mixing unit, a gaseous raw material feeding device and a feeding method, which can uniformly premix gaseous silicon-containing raw materials and gaseous titanium-containing raw materials in advance in a tank body according to a fixed mass ratio, do not condense, can ensure that the mass fraction of each component in mixed particles of silicon dioxide and titanium dioxide deposited on a deposition surface is fixed, the components are uniform, the deposition rate is stable, and the titanium-doped quartz glass with extremely low thermal expansion coefficient and higher optical uniformity can be prepared.
The technical scheme adopted by the invention is as follows:
a bulk blending unit comprising a first feed conduit and a second feed conduit for transporting a gaseous silicon-containing feedstock and a gaseous titanium-containing feedstock, respectively, the bulk blending unit further comprising: the tank body is a main mixing area of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material at a preset mixing temperature, so as to form a mixed gas which is fixed in mass fraction of each component, uniformly mixed and free from condensation; the first material conveying pipeline and the second material conveying pipeline are respectively connected with the tank body, and a gaseous silicon-containing raw material and a gaseous titanium-containing raw material are input into the tank body according to a preset proportion, and the temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material when entering the tank body reaches a preset mixing temperature;
a mixing output pipe connected with the tank to guide the mixed gas in the tank to a burner;
the compensating gas input pipeline is connected with the tank body, compensating gas is input into the tank body according to a preset proportion, and the temperature of the compensating gas when entering the tank body is higher than a preset mixing temperature so as to compensate preset mixing temperature fluctuation caused when the gaseous silicon-containing raw material and the gaseous titanium-containing raw material enter the tank body for premixing, so that condensation and dew condensation of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in the tank body are avoided;
wherein the volume of the tank body is larger than the sum of the volumes of the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas which are input in the specified time; the pressure in the tank body is smaller than the pressure in the first material conveying pipeline, the second material conveying pipeline and the compensating gas input pipeline.
Further, the connection parts of the first material conveying pipeline and the second material conveying pipeline and the tank body are respectively provided with one-way valves.
Further, a heat tracing belt is arranged on the first material conveying pipeline;
and/or a heat tracing belt is arranged on the second material conveying pipeline;
and/or the compensation gas input pipeline is provided with a heat tracing belt
And/or a heat tracing band is arranged on the mixed output pipeline.
Further, a stirrer is also arranged in the tank body.
Further, the direction of the gaseous silicon-containing raw material in the first material conveying pipeline entering the tank body, the direction of the gaseous titanium-containing raw material in the second material conveying pipeline entering the tank body and the direction of the compensating gas in the compensating gas conveying pipeline entering the tank body are not all overlapped or different.
Further, the tank body is connected with a safety pipeline; the safety pipeline is provided with a safety valve and a flame arrester, and the SV615 British Sipessary safety valve, DN30 and 316SS are used for tank overpressure protection; the German Rockwell CNG flame arrester is in threaded connection and is used for preventing tempering when mixed gas is discharged at high altitude.
Based on the same inventive concept, the invention also provides a gaseous raw material feeding device for preparing zero-expansion titanium-doped quartz glass, which comprises a silicon-containing raw material electric heating evaporation cabinet, a titanium-containing raw material electric heating evaporation cabinet and a PLC controller, and is characterized by further comprising a compensation gas electric heating evaporation cabinet and the above-mentioned body-increasing mixing unit; the silicon-containing raw material electric heating evaporation cabinet, the titanium-containing raw material electric heating evaporation cabinet and the compensation gas electric heating evaporation cabinet are respectively connected with a first material conveying pipeline, a second material conveying pipeline and a compensation gas input pipeline of the body-increasing mixing unit; the PLC is electrically connected with the silicon-containing raw material electric heating evaporation cabinet, the titanium-containing raw material electric heating evaporation cabinet and the compensation gas electric heating evaporation cabinet.
Further, the gaseous raw material feeding device further comprises a filter; the filter is respectively arranged on the first material conveying pipeline and the second material conveying pipeline, or the filter is respectively arranged on the first material conveying pipeline, the second material conveying pipeline and the compensation gas input pipeline.
Based on the same inventive concept, the invention also provides a gaseous raw material feeding method for preparing the zero-expansion titanium-doped quartz glass, which is implemented based on the gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass, and comprises the following steps:
heating a silicon-containing raw material and a titanium-containing raw material respectively to generate a gaseous silicon-containing raw material and a gaseous titanium-containing raw material;
heating the compensation gas;
inputting the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas into a tank body according to a preset proportion, and mixing; controlling the temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material when entering the tank body to be a preset mixing temperature; controlling the temperature of the compensation gas when entering the tank body to be higher than the preset mixing temperature; the pressure in the control tank body is smaller than the pressure in the first material conveying pipeline, the second material conveying pipeline and the compensation gas input pipeline;
after the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are mixed, the mixed gas with fixed mass fractions of all components in the gas is obtained, the mixed gas is uniformly mixed and does not generate condensation dew, and the mixed gas is used as carrier gas to be led into a burner.
Further, the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas which are respectively gaseous SiCl are input into the tank body 4 Gaseous TiCl 4 And hydrogen.
Further, gaseous SiCl is added up to 100% by mass ratio 4 Gaseous TiCl 4 And H 2 The mass percentages of the components are 88-93%, 5-10% and the balance respectively.
Further, gaseous SiCl 4 And gaseous TiCl 4 The temperature when entering the tank body is 135-140 ℃; h 2 The temperature of the water entering the tank body is 145-150 ℃.
The beneficial effects of the invention are as follows:
1. the invention provides a bulk-increasing mixing unit. The adding mixing unit is added with a tank body and a compensating gas input pipeline, and in the tank body, the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are premixed in advance; meanwhile, the compensation gas is input by using a compensation gas input pipeline to compensate the temperature fluctuation of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material during the premixing of the tank body. On the basis, the method can realize that the raw materials containing silicon and titanium in a state are uniformly premixed in the tank body according to a fixed mass ratio in advance, and condensation and dew do not occur.
2. The invention also provides a gaseous raw material feeding device and a feeding method for preparing the zero-expansion titanium-doped quartz glass, which can provide SiCl with fixed mass fractions, uniform mixing and fixed flow of each component for the combustor 4 And TiCl 4 And (3) mixing gas. Due to gaseous SiCl arranged in preset proportions 4 And gaseous TiCl 4 The tank body of the body-increasing mixing unit in the gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass is premixed in advance, and meanwhile, the body-increasing mixing unit in the gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass provided by the invention is provided with a compensating gas input pipeline, and the compensating gas is utilized to premix gaseous SiCl in the tank body 4 And gaseous TiCl 4 To compensate for temperature fluctuations in (a). On the basis, gaseous SiCl can be realized 4 And gaseous TiCl 4 The silicon dioxide and titanium dioxide mixed particles are uniformly premixed in the tank body according to a fixed mass ratio in advance, condensation dew is not generated, the mass fraction of each component in the mixed particles of silicon dioxide and titanium dioxide deposited on the deposition surface is ensured to be fixed, the components are uniform, the deposition rate is stable, and the doped with higher optical uniformity can be preparedTitanium quartz glass.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments of the present application will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of an additional mixing unit in embodiment 1 of the present application;
FIG. 2 is a schematic structural view of a manufacturing apparatus of zero-expansion silica glass in example 2 of the present application;
FIG. 3 SiCl in example 3 of the present application 4 Vapor pressure versus temperature curve and TiCl 4 Vapor pressure versus temperature curve;
FIG. 4 TiCl in example 3 of the present application 4 -SiCl 4 A gas-liquid phase diagram of a binary system.
Description of the embodiments
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in numerous different ways without departing from the spirit or scope of the embodiments of the present application. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
The terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the embodiments of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the embodiments of the present application, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and the like are to be construed broadly, and may be directly connected or indirectly connected through intermediaries, for example, in communication between two elements or in an interaction relationship between the two elements. The specific meaning of the above terms in the embodiments of the present application will be understood by those of ordinary skill in the art according to the specific circumstances.
Example 1
As shown in fig. 1, in this embodiment, a bulk-increasing mixing unit is provided for uniformly premixing two gaseous raw materials for preparing titanium-doped quartz glass in advance in a tank 1 according to a fixed mass ratio, and condensation and dew condensation do not occur in the process of transferring from the tank 1 to a burner 8 before and after premixing in the tank 1.
The bulk-increasing mixing unit comprises a first material conveying pipeline 2 and a second material conveying pipeline 3. The first feed conveying pipeline 2 and the second feed conveying pipeline 3 are conveying pipelines of gaseous silicon-containing raw materials and gaseous titanium-containing raw materials respectively. In addition, in order to ensure that the gaseous silicon-containing raw material and the gaseous titanium-containing raw material respectively maintain a gaseous state in the process of conveying the first conveying pipeline 2 and the second conveying pipeline 3, heat insulation layers (such as asbestos) are wrapped on the outer walls of the first conveying pipeline 2 and the second conveying pipeline 3 so as to reduce heat loss. By increasing the pressure of the feed to the first feed transfer line 2 and the second feed transfer line 3 and maintaining the temperature in the lines, the dew point temperature of the gaseous silicon-containing feedstock and the gaseous titanium-containing feedstock can be increased, preventing condensation of the gaseous silicon-containing feedstock and the gaseous titanium-containing feedstock.
The gaseous silicon-containing raw material and the gaseous titanium-containing raw material are condensed in the mixing process, mainly because the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are in contact with each other, the gaseous silicon-containing raw material causes the gaseous titanium-containing raw material to be condensed in a small degree, or the gaseous titanium-containing raw material causes the gaseous silicon-containing raw material to be condensed in a small degree. In order to mix the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in advance and prevent condensation of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material during the mixing process, the bulk mixing unit further comprises a tank 1, a mixing output pipe 5 and a compensating gas input pipe 4 in this embodiment. The tank 1 is a main mixing area of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material at a preset mixing temperature. As shown in fig. 1, the tank 1 has a hollow cylindrical structure as a whole. An insulating layer or a jacket heating layer is arranged on the outer wall of the tank body 1 so as to reduce heat dissipation of the tank body 1 and maintain the temperature in the tank body 1. The first material conveying pipeline 2 and the second material conveying pipeline 3 are positioned at one end of the tank body 1 in the axial length direction. The first and second feed delivery pipes 2 and 3 are communicated with the hollow interior of the tank 1 to introduce the gaseous silicon-containing raw material and the gaseous titanium-containing raw material into the tank 1, respectively, in a predetermined ratio. The mixing output pipeline 5 is positioned at the other end of the tank body 1 in the axial length direction. The mixing output pipe 5 is a conveying pipe of a mixed gas formed by mixing the gaseous silicon-containing raw material and the gaseous titanium-containing raw material so as to guide the mixed gas to the burner 8. And, also wrap up and be provided with heat preservation (such as asbestos) on the outer wall of mixing output pipeline 5 to reduce the heat loss, prevent gaseous silicon-containing raw materials and gaseous titanium-containing raw materials to take place the condensation. The make-up gas input pipe 4 is also communicated with the hollow interior of the tank 1 to input the heated make-up gas (oxygen or hydrogen) to the tank 1 in a predetermined ratio. The temperature of the compensation gas when entering the tank body 1 is higher than the preset mixing temperature, so that the temperature fluctuation generated in the process of contacting and mixing the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in the tank body 1 can be compensated, and condensation and dew formation of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in the tank body 1 can be avoided. An insulating layer (such as asbestos) is also wrapped on the outer wall of the compensator input pipeline 4 to reduce heat loss and maintain the temperature of the compensating gas.
Since the gaseous silicon-containing raw material and the gaseous titanium-containing raw material have different vapor pressures before being conveyed to the tank 1 along the first conveying pipeline 2 and the second conveying pipeline 3, respectively. The volume of the tank 1 should be larger than the sum of volumes of the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas respectively input by the first conveying pipeline 2, the second conveying pipeline 3 and the compensating gas input pipeline 4 in a prescribed time. When the gaseous silicon-containing raw material and the gaseous titanium-containing raw material with preset proportions enter the tank body 1, the first material conveying pipeline 2 and the second material conveying pipeline 3 are used for restraining the gaseous silicon-containing raw material and the gaseous titanium-containing raw material to disappear, the gaseous silicon-containing raw material and the gaseous titanium-containing raw material instantly release pressure, so that temperature fluctuation can be generated, and the compensating gas synchronously input into the tank body 1 according to the preset proportions is used for compensating the temperature fluctuation of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material, so that the mixed gas with fixed mass fractions of all components in the tank body 1, uniform mixing and no condensation and dew are formed after the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are mixed. At the same time, the make-up gas also acts as a carrier gas to direct the mixed gas stream to the burner 8. And the pressure in the tank body 1 is smaller than the pressure of the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas which are respectively input into the tank body 1 by the first material conveying pipeline 2, the second material conveying pipeline 3 and the compensating gas input pipeline 4, so that the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas can be normally fed.
In this embodiment, the connection parts of the first material conveying pipeline 2 and the second material conveying pipeline 3 and the tank body 1 are respectively provided with a one-way valve 9, so that the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are respectively limited to flow into the tank body 1 in one way only, and the mixed gas in the tank body 1 is prevented from flowing backwards.
In this embodiment, a plurality of heat tracing bands 10 are disposed on the first conveying pipeline 2 and the second conveying pipeline 3, so as to gradually heat the gaseous silicon-containing raw material conveyed in the first conveying pipeline 2 and the gaseous titanium-containing raw material conveyed in the second conveying pipeline 3 to a preset mixing temperature. A heat tracing band 10 is also provided on the make-up gas input pipe 4 to maintain the temperature of the make-up gas above the preset mixing temperature. The mixing output pipe 5 is also provided with a heat tracing belt 10 to further heat the mixed gas gradually to a preset feeding temperature. Meanwhile, when the gaseous silicon-containing raw material conveyed in the first conveying pipeline 2 and the gaseous titanium-containing raw material conveyed in the second conveying pipeline 3 are gradually heated to a preset mixing temperature by the heat tracing belt 10, the dew point temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material is favorably improved by matching with the conveying pressure in the gaseous silicon-containing raw material conveyed in the first conveying pipeline 2 and the conveying pressure in the second conveying pipeline 3, and the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are prevented from being condensed.
For example, a heat tracing band 10 is provided near the start end, near the middle section and near the end of the first transfer pipe 2 in the transfer direction, respectively, to gradually raise the temperature of the gaseous silicon-containing raw material from 100 ℃ to 140 ℃. A heat tracing band 10 is provided near the start end, near the middle section and near the end of the second conveying pipeline 3 in the conveying direction, respectively, to gradually raise the temperature of the gaseous titanium-containing raw material from 135 ℃ to 140 ℃. A heat tracing band 10 is provided near the middle section of the mixing output pipe 5 to raise the temperature of the mixture from 140 c to 145 c. Hydrogen is selected as compensation gas, and a heat tracing belt 10 is respectively arranged near the initial end and near the middle section on the compensation gas input pipeline 4 so as to maintain the temperature of the hydrogen at 150 ℃.
In this embodiment, in order to increase the speed of uniformly mixing the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in the tank 1, a stirrer 6 is further provided in the tank 1. The agitator 6 is rotated by a motor. When the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are conveyed to the tank body 1, the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are rapidly and uniformly dispersed under the stirring action of the stirrer 6, so that the uniform mixing efficiency of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material is improved.
In this embodiment, the direction in which the compensation gas input pipeline 4 introduces hydrogen into the tank 1 intersects with the connection direction of the first and second delivery pipelines 2 and 3 and the mixing output pipeline 5, so that the compensation gas can provide a certain assistance for mixing the gaseous silicon-containing raw material and the gaseous titanium-containing raw material, and accelerate the process of uniform mixing. For example, the make-up gas input pipe 4 is provided in a tangential direction of the circumferential outer wall of the tank 1, whereby the hydrogen gas can form a circular flow within the tank 1.
In this embodiment, the bulk mixing unit further comprises a safety conduit 7 for ensuring operational safety. The safety pipeline 7 is communicated with the hollow inside of the tank body 1. A safety valve 11 and a flame arrester 12 are provided on the safety line 7. When the pressure of the tank 1 increases due to an emergency, the mixed gas or the like can be safely discharged through the safety pipe 7.
The working mode of the body-increasing mixing unit is as follows: according to the preset proportion, the first material conveying pipeline 2 conveys the gaseous silicon-containing raw material, the second material conveying pipeline 3 conveys the gaseous titanium-containing raw material, and the compensating gas conveying pipeline 4 conveys the compensating gas. The temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material when entering the tank 1 is a preset mixing temperature. The temperature of the hydrogen gas when entering the tank 1 is higher than the preset mixing temperature. The stirrer 6 is driven by a motor to stir and mix the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in the tank body 1 to form a premixed, non-condensing and saturated mixed gas. The finally and uniformly mixed gas is output by a mixing output pipeline 5 and is led to a combustor 8.
Example 2
On the basis of the bulk mixing unit in example 1, a gaseous raw material feeding device for the preparation of zero-expansion titanium-doped quartz glass is provided in this example to provide a uniformly mixed mixture to the burner 8.
The gaseous raw material feeding device comprises a silicon-containing raw material electric heating evaporation cabinet, a titanium-containing raw material electric heating evaporation cabinet, a compensation gas electric heating evaporation cabinet, a PLC controller and a body-increasing mixing unit. The structure of the bulk mixing unit is the same as described in example 1. The silicon-containing raw material electric heating evaporation cabinet and the titanium-containing raw material electric heating evaporation cabinet are respectively communicated with the starting ends of the first conveying pipeline 2 and the second conveying pipeline 3. The compensation gas electric heating evaporation cabinet is communicated with the starting end of the compensation gas input pipeline 4. The tank body 1, the first material conveying pipeline 2, the second material conveying pipeline 3, the mixed output pipeline 5 and the compensating gas input pipeline 4 are also provided with an electronic thermometer and an electronic pressure gauge. The PLC is electrically connected with motors of the silicon-containing raw material electric heating evaporation cabinet, the titanium-containing raw material electric heating evaporation cabinet, the compensation gas electric heating evaporation cabinet, the electronic thermometer, the electronic pressure gauge, the heat tracing belt 10 and the stirrer 6. The PLC controls the heating temperatures of the silicon-containing raw material electric heating evaporation cabinet, the titanium-containing raw material electric heating evaporation cabinet and the compensation gas electric heating evaporation cabinet to generate gaseous silicon-containing raw materials, gaseous titanium-containing raw materials and high-temperature compensation gas, and the gaseous silicon-containing raw materials, the gaseous titanium-containing raw materials and the high-temperature compensation gas are respectively led into the tank body 1 through the first material conveying pipeline 2, the second material conveying pipeline 3 and the compensation gas input pipeline 4. The PLC controls the stirrer 6 to rotate, so that the gaseous silicon-containing raw materials and the gaseous titanium-containing raw materials are quickly and uniformly mixed into the mixed gas which is fixed in mass fraction of each component in the gas, uniformly mixed and free from condensation and dew. The mixed gas is then used as carrier gas and led to the burner 8 through the mixed output pipeline 5. Meanwhile, the PLC controller dynamically regulates and controls the evaporation and mixing processes according to the flow, the temperature and the pressure detected by the electronic thermometer and the electronic pressure meter.
The gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass provided in the embodiment can provide the burner 8 with fixed mass fractions of the components insideUniformly mixed SiCl with fixed flow 4 And TiCl 4 And (3) mixing gas. Due to gaseous SiCl arranged in preset proportions 4 And gaseous TiCl 4 The tank 1 of the bulk mixing unit in the gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass is premixed in advance, and meanwhile, the bulk mixing unit in the gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass provided by the invention is provided with a compensating gas input pipeline, and the compensating gas is utilized to premix gaseous SiCl in the tank 1 4 And gaseous TiCl 4 To compensate for temperature fluctuations in (a). On the basis, gaseous SiCl can be realized 4 And gaseous TiCl 4 The titanium doped quartz glass with higher optical uniformity and zero expansion is prepared by uniformly premixing the silicon dioxide and titanium dioxide in the tank body 1 according to a fixed proportion in advance, and not generating condensation dew, and can ensure that the mass fraction of each component in the mixed particles of the silicon dioxide and titanium dioxide deposited on a deposition surface is fixed, the components are uniform and the deposition rate is stable.
In this embodiment, the gaseous raw material supply device includes a filter in order to reduce the influence of impurities in the gaseous silicon-containing raw material, the gaseous titanium-containing raw material, and the like. Filters are respectively arranged on the first conveying pipeline 2 and the second conveying pipeline 3 to filter impurities of the gaseous silicon-containing raw materials and the gaseous titanium-containing raw materials and improve the purity of the gaseous silicon-containing raw materials and the gaseous titanium-containing raw materials. Further, a filter may be disposed on the compensation gas input pipe 4 to filter impurities in the compensation gas, so as to improve the purity of the compensation gas.
Example 3
Based on the gaseous raw material feeding device for preparing the zero-expansion titanium-doped quartz glass in the embodiment 2, the gaseous raw material feeding method for preparing the zero-expansion titanium-doped quartz glass comprises the following steps:
heating a silicon-containing raw material and a titanium-containing raw material respectively to generate a gaseous silicon-containing raw material and a gaseous titanium-containing raw material;
heating the compensation gas;
inputting the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas into the tank body 1 according to a preset proportion, and mixing; controlling the temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material when entering the tank body 1 to be a preset mixing temperature; controlling the temperature of the compensation gas when entering the tank body 1 to be higher than the preset mixing temperature; the pressure in the control tank body 1 is smaller than the pressure in the first material conveying pipeline 2, the second material conveying pipeline 3 and the compensating gas input pipeline 4;
after the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are mixed, the mixed gas which has fixed mass fractions of each component, is uniformly mixed and does not generate condensation dew is obtained, and the mixed gas is used as carrier gas to be led into the next working procedure.
The following is SiCl 4 And TiCl 4 The preparation of the titanium doped quartz glass is specifically described by taking hydrogen as a compensation gas as an example, and mainly comprises the following steps:
step (1), heating liquid SiCl respectively 4 And liquid TiCl 4 Evaporating to obtain gaseous SiCl 4 And gaseous TiCl 4 . At this time, gaseous SiCl 4 Is 100 ℃, gaseous TiCl 4 The temperature of (2) was 135 ℃.
Step (2) of evaporating the vapor to obtain gaseous SiCl 4 Gradually heating from 100 ℃ to 140 ℃; synchronously evaporating and vaporizing to obtain gaseous TiCl 4 Is gradually heated from 135 ℃ to 140 ℃.
Step (3), the gaseous SiCl after the synchronous temperature rising in the step (2) is processed 4 Gaseous TiCl 4 And delivering the hydrogen at 150 ℃ into the tank body 1 of the bulk mixing unit to obtain mixed gas which has fixed mass fractions of the components, is uniformly mixed and does not generate condensation, and introducing the mixed gas into the next process by taking the hydrogen as carrier gas.
Wherein, the total mass ratio is 100 percent, the gaseous SiCl is input into the tank body 1 4 Gaseous TiCl 4 And H 2 The mass percentages of the components are 88-93%, 5-10% and the balance respectively.
SiCl can be obtained according to the Clavipitalong equation 4 Saturated vapor pressure versus temperature curve and TiCl 4 The saturation vapor pressure versus temperature curve is shown in figure 3.
According to Laurager's law and Dalton partial pressure law, calculate different valuesTiCl at mole fraction 4 -SiCl 4 At different temperatures, the bubble point and dew point, tiCl is obtained 4 -SiCl 4 The gas-liquid phase diagram of the binary system is shown in fig. 4. As can be seen from the figures, tiCl is controlled 4 -SiCl 4 The mixing ratio and the mixing temperature of (2) can be such that gaseous TiCl 4 And gaseous SiCl 4 A non-condensing state is achieved in the tank 1.
At this time, it is assumed that the gas composition of the can 1 is shown in Table 1, and the can 1 has a volume ofVAt a temperature ofT。
The molar mass of the gas mixture in the tank 1 is:
M=M 1 ×y 1 +M 2 ×y 2 +M 3 ×y 3
wherein H is 2 : molar mass ofM 1 Mole fraction ofy 1 ；SiCl 4 : molar mass ofM 2 Mole fraction ofy 2 ；TiCl 4 : molar mass ofM 3 Mole fraction ofy 3 The method comprises the steps of carrying out a first treatment on the surface of the Calculation of the molar mass of the Mixed gasM63.66 or 61.4.
TABLE 1-2 ratio of the components of the gas mixture in tank 1
According to Avgalde Luo Dinglv, the total pressure of the mixture in the tank 1 is knownPThe method comprises the following steps:
suppose H 2 Is respectively the mass and the volume flow rate ofm 1 Andq v1 ；SiCl 4 is respectively the mass and the volume flow rate ofm 2 Andq v2 ；TiCl 4 is respectively the mass and the volume flow rate ofm 3 Andq v3 the method comprises the steps of carrying out a first treatment on the surface of the MixingThe total gas pressure is:
or:
when (when)MWhen the value of the component is =63.66,q v1 is 3 to 5slm in length and is made of a material,q v2 is 6 to 10slm in length,q v3 0.5 to 2slm;
or whenMWhen the number of the samples is =61.4,q v1 is 3 to 5slm in length and is made of a material,q v2 is 6 to 10slm in length,q v3 0.5 to 2slm;
assuming a pipeline gas volume ofV*At a temperature ofT*The air pressure of each pipeline is as follows:
taking hydrogen as an example for pipeline pressurePressure with mixerPSize relationship:
due toTAnd (3) withT*Controllable andV*and (3) withVControllable, make:
thenIn the same way, can realize->，/>。
In combination, the first material conveying pipeline 2, the second material conveying pipeline 3 and the compensating gas input pipeline 4 are all larger than the total pressure value in the tank body 1, so that the gaseous SiCl is input into the tank body 1 through the first material conveying pipeline 2, the second material conveying pipeline 3 and the compensating gas input pipeline 4 4 Gaseous TiCl 4 And hydrogen requirements.
Claims (12)
1. A bulk blending unit comprising a first feed conduit and a second feed conduit for transporting a gaseous silicon-containing feedstock and a gaseous titanium-containing feedstock, respectively, the bulk blending unit further comprising:
the tank body is a main mixing area of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material at a preset mixing temperature so as to form a mixed gas with fixed mass fractions of all components in the tank body, uniform mixing and no condensation; the first material conveying pipeline and the second material conveying pipeline are respectively connected with the tank body, and a gaseous silicon-containing raw material and a gaseous titanium-containing raw material are input into the tank body according to a preset proportion, and the temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material when entering the tank body reaches a preset mixing temperature;
a mixing output pipe connected with the tank to guide the mixed gas in the tank to a burner;
the compensating gas input pipeline is connected with the tank body, compensating gas is input into the tank body according to a preset proportion, and the temperature of the compensating gas when entering the tank body is higher than a preset mixing temperature so as to compensate preset mixing temperature fluctuation caused when the gaseous silicon-containing raw material and the gaseous titanium-containing raw material enter the tank body for premixing, so that condensation and dew condensation of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material in the tank body are avoided;
wherein the volume of the tank body is larger than the sum of the volumes of the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas which are input in the specified time; the pressure in the tank body is smaller than the pressure in the first material conveying pipeline, the second material conveying pipeline and the compensating gas input pipeline.
2. The bulk-increasing mixing unit of claim 1, wherein the first and second material-conveying pipelines are provided with one-way valves at the connection points with the tank, respectively.
3. The bulk-increasing mixing unit of claim 1, wherein a heat trace strip is disposed on the first feed conduit;
and/or a heat tracing belt is arranged on the second material conveying pipeline;
and/or the compensation gas input pipeline is provided with a heat tracing belt
And/or a heat tracing band is arranged on the mixed output pipeline.
4. The add-on mixing unit of claim 1, wherein a stirrer is also provided within the tank.
5. The bulk blending unit of claim 1, wherein the direction of gaseous silicon-containing feedstock in the first feed conduit into the tank, the direction of gaseous titanium-containing feedstock in the second feed conduit into the tank, and the direction of compensating gas in the compensating gas feed conduit into the tank are not all coincident or different.
6. The add-on mixing unit of claim 1, wherein the tank is further connected with a safety conduit; the safety pipeline is provided with a safety valve and a flame arrester.
7. A gaseous raw material feeding device for preparing zero-expansion titanium-doped quartz glass, which comprises a silicon-containing raw material electric heating evaporation cabinet, a titanium-containing raw material electric heating evaporation cabinet and a PLC (programmable logic controller), and is characterized by further comprising a compensation gas electric heating evaporation cabinet and the body-increasing mixing unit according to any one of claims 1-6; the silicon-containing raw material electric heating evaporation cabinet, the titanium-containing raw material electric heating evaporation cabinet and the compensation gas electric heating evaporation cabinet are respectively connected with a first material conveying pipeline, a second material conveying pipeline and a compensation gas input pipeline of the body-increasing mixing unit; the PLC is electrically connected with the silicon-containing raw material electric heating evaporation cabinet, the titanium-containing raw material electric heating evaporation cabinet and the compensation gas electric heating evaporation cabinet.
8. The gaseous raw material feeding device for producing zero-expansion titanium-doped silica glass according to claim 7, further comprising a filter; the filter is respectively arranged on the first material conveying pipeline and the second material conveying pipeline, or the filter is respectively arranged on the first material conveying pipeline, the second material conveying pipeline and the compensation gas input pipeline.
9. A gaseous raw material feeding method for the production of zero-expansion titanium-doped quartz glass, implemented on the basis of a gaseous raw material feeding device for the production of zero-expansion titanium-doped quartz glass according to claim 7 or 8, characterized in that the gaseous raw material feeding method comprises the steps of:
heating a silicon-containing raw material and a titanium-containing raw material respectively to generate a gaseous silicon-containing raw material and a gaseous titanium-containing raw material;
heating the compensation gas;
inputting the gaseous silicon-containing raw material, the gaseous titanium-containing raw material and the compensating gas into a tank body according to a preset proportion, and mixing; controlling the temperature of the gaseous silicon-containing raw material and the gaseous titanium-containing raw material when entering the tank body to be a preset mixing temperature; controlling the temperature of the compensation gas when entering the tank body to be higher than the preset mixing temperature; the pressure in the control tank body is smaller than the pressure in the first material conveying pipeline, the second material conveying pipeline and the compensation gas input pipeline;
after the gaseous silicon-containing raw material and the gaseous titanium-containing raw material are mixed, the mixed gas which has fixed mass fractions of all components in the gas, is uniformly mixed and does not generate condensation dew is obtained, and the mixed gas is used as carrier gas to be led into a burner.
10. The method for feeding a gaseous raw material for producing a zero-expansion titanium-doped silica glass according to claim 9, wherein the gaseous raw material containing silicon, the gaseous raw material containing titanium and the compensating gas fed into the tank are gaseous SiCl, respectively 4 Gaseous TiCl 4 And hydrogen.
11. The method for producing a zero-expansion titanium-doped silica glass according to claim 10, wherein the gaseous SiCl is added up to 100% by mass 4 Gaseous TiCl 4 And H 2 The mass percentages of the components are 88-93%, 5-10% and the balance respectively.
12. The method for feeding a gaseous raw material for producing zero-expansion titanium-doped silica glass according to claim 10, wherein the gaseous SiCl 4 And gaseous TiCl 4 The temperature when entering the tank body is 135-140 ℃; h 2 The temperature of the water entering the tank body is 145-150 ℃.
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