CN110371990A - A kind of hydrolysis furnace producing fumed silica and system - Google Patents
A kind of hydrolysis furnace producing fumed silica and system Download PDFInfo
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- CN110371990A CN110371990A CN201910591145.6A CN201910591145A CN110371990A CN 110371990 A CN110371990 A CN 110371990A CN 201910591145 A CN201910591145 A CN 201910591145A CN 110371990 A CN110371990 A CN 110371990A
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- 230000007062 hydrolysis Effects 0.000 title claims abstract description 102
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 102
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910021485 fumed silica Inorganic materials 0.000 title claims abstract description 63
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 206
- 239000001257 hydrogen Substances 0.000 claims abstract description 196
- 239000003570 air Substances 0.000 claims abstract description 78
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 67
- 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 claims abstract description 59
- 238000004519 manufacturing process Methods 0.000 claims abstract description 37
- -1 DCS control system Chemical compound 0.000 claims abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 184
- 239000007789 gas Substances 0.000 claims description 100
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 88
- 239000001301 oxygen Substances 0.000 claims description 88
- 229910052760 oxygen Inorganic materials 0.000 claims description 88
- 230000001105 regulatory effect Effects 0.000 claims description 58
- 150000002431 hydrogen Chemical class 0.000 claims description 22
- 238000003556 assay Methods 0.000 claims description 20
- 238000012360 testing method Methods 0.000 claims description 18
- 238000001514 detection method Methods 0.000 claims description 12
- 230000009467 reduction Effects 0.000 claims description 11
- 230000008901 benefit Effects 0.000 claims description 10
- 230000007246 mechanism Effects 0.000 claims description 9
- 230000002238 attenuated effect Effects 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 239000013589 supplement Substances 0.000 claims description 4
- 238000004868 gas analysis Methods 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 230000008569 process Effects 0.000 description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000000460 chlorine Substances 0.000 description 10
- 229910052801 chlorine Inorganic materials 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 10
- 238000011282 treatment Methods 0.000 description 9
- 238000007600 charging Methods 0.000 description 8
- 230000003301 hydrolyzing effect Effects 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 229910003978 SiClx Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 239000005708 Sodium hypochlorite Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000006392 deoxygenation reaction Methods 0.000 description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The present invention discloses a kind of hydrolysis furnace for producing fumed silica, including DCS control system, it further include temperature control unit, pressure control unit, temperature control unit is used to detect the temperature of the flame generated in hydrolysis furnace, and the inlet amount of silicon tetrachloride, hydrogen, air is adjusted according to the temperature detected；Pressure control unit is connect with the furnace tube of hydrolysis furnace, for adjusting the pressure in hydrolysis furnace, to control the residence time in flame of the fumed silica generated.Invention additionally discloses a kind of systems of production fumed silica containing hydrolysis furnace described above.The present invention can be precisely controlled flame temperature, the pressure in hydrolysis furnace, obtain that partial size is small, fumed silica product of large specific surface area.
Description
Technical field
A kind of system present invention relates particularly to hydrolysis furnace for producing fumed silica and containing the hydrolysis furnace.
Background technique
Fumed silica is a kind of important nano inorganic chemical materials, and partial size is small (7-40nm), large specific surface area
(50-600 ㎡/g), have superior surface chemistry, silicon rubber, adhesive, paint, coating, sealing material, ink,
The fields such as electronics, paper, cosmetics, medicine, food, agricultural and CMP have a wide range of applications.
The preparation of fumed silica is mainly hydrolyzed under 1800 DEG C of hot conditions using silicon tetrachloride, process are as follows:
Under the high temperature conditions, firstly, the oxygen in air reacts in the presence of silicon tetrachloride with hydrogen generates water, then water and tetrachloro
SiClx hydrolyzes, and reactional equation is as follows:
2H2+O2+SiCl4——→SiO2+4HCl
In this reaction process, the factors such as flame temperature, fumed silica residence time (related with furnace pressure) are all
It will affect the granularity, specific surface area and surface nature of silica, therefore, how to accurately control flame temperature, furnace pressure is
Prepare the key of the fumed silica of high quality.And in the production equipment of current fumed silica, there are it is following not
Foot:
(1) control temperature: the burner flame temperature of existing hydrolysis furnace is detected using thermocouple, is generated in burner
The deep-etchings such as hydrogen chloride, chlorine, strong oxidizing property gas can generate serious corrosion and oxidation to thermocouple, hold thermocouple
It is easy to damage, cause temperature measurement not accurate, can not judge whether the flame temperature of burner reaches 1800 DEG C, to can not judge to give birth to
The quality of the fumed silica of production, therefore, it is necessary to adjust gas further according to product quality to product sampling analysis product quality
State silicon tetrachloride, hydrogen, air feed amount, to control the flame temperature of burner, this mode leads to temperature control lag, produces
Product specific surface area is difficult to be optimal, and product quality is unable to get guarantee, and complicated for operation, heavy workload, brings to production huge
It is big inconvenient.
(2) pressure controls: at a suitable temperature, the fumed silica that hydrolyzing silicon tetrachloride generates stops in flame
Time it is shorter, specific surface area is bigger, and influencing the residence time is negative pressure in furnace, and negative pressure is high to will cause material unstable combustion
Fixed, the low fumed silica residence time in flame that will cause of negative pressure is longer (more than 1.5S), causes under specific surface area
Drop, but vacuum cavitations are unstable in existing hydrolysis furnace, it is difficult to maintain suitable condition of negative pressure.
(3) tail gas controls: during hydrolyzing silicon tetrachloride, in order to guarantee that silicon tetrachloride sufficiently reacts, excess need to be added
Oxygen, but excessive oxygen is under furnace high-temperature environment, and the reaction was continued for the hydrogen chloride that can be generated with hydrolysis, output chlorine
Gas, chlorine are toxic gas, so that increase the chlorine treatments processes such as lye absorbs, sodium hypochlorite is handled in subsequent handling, with
The processing for guaranteeing the toxic gases such as chlorine, increases operating cost.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of production gas phase two for the above deficiency of the existing technology
The hydrolysis furnace and system of silica can be precisely controlled temperature, the pressure of flame in hydrolysis furnace, obtain partial size it is small,
The fumed silica product of large specific surface area.
According to an aspect of the present invention, the hydrolysis furnace of production fumed silica is provided, its technical solution is as follows:
A kind of hydrolysis furnace producing fumed silica, including furnace body, the furnace body include burner and furnace tube, the hydrolysis
Furnace further includes that (i.e. dcs Distributed Control System is adopted based on microprocessor to DCS
It concentrated, taken into account point with control function dispersion, display operation and the instrument of new generation of autonomous and comprehensive coordination design principle controls
System) control system, temperature control unit, pressure control unit,
The DCS control system for centralized control and coordinates temperature control unit, pressure control unit and tail gas group
Divide control unit；
The temperature control unit includes temperature measurer, feeding mechanism, and the temperature measurer is set on the furnace body, and with it is described
The electrical connection of DCS control system, for detecting the temperature of the flame generated in furnace body, and the temperature information that will test is transferred to
DCS control system；Temperature threshold is equipped in the DCS control system, DCS control system is used for the temperature for detecting temperature measurer
Information is compared with the temperature threshold, and calculates the inlet amount of silicon tetrachloride, hydrogen, air, then transmits these chargings
Measure information；The feeding mechanism is connect with the furnace body, is also electrically connected with the DCS control system, is controlled according to the DCS received
The inlet amount information that system processed passes out is passed through silicon tetrachloride, hydrogen and air into furnace body；
The pressure control unit is connect with the furnace tube of the furnace body, and is electrically connected with the DCS control system, for adjusting
The intracorporal pressure of furnace is saved, to control residence time of the fumed silica generated in flame.
Preferably, the feeding mechanism includes silicon tetrachloride feeding component, hydrogen feeding assembly, air feed component,
The silicon tetrachloride feeding component includes silicon tetrachloride feeding pipeline, first flowmeter, the first regulating valve, and described four
Silicon chloride feeding line is connect with the burner of the furnace body, and the first flowmeter and first regulating valve are set to tetrachloro
On silicon feeding line, and first flowmeter and the first regulating valve are electrically connected with the DCS control system, and the first regulating valve is used for
Itself aperture is adjusted according to the inlet amount of the silicon tetrachloride set in DCS control system, to control the inlet amount of silicon tetrachloride, the
Flow meters are for measuring the amount for being passed into the intracorporal silicon tetrachloride of furnace；
The hydrogen feeding assembly includes hydrogen feed line, second flowmeter, the second regulating valve, the hydrogen feed tube
Line is connect with the burner of the furnace body, and the second flowmeter and second regulating valve are set in hydrogen feed line, and
Second flowmeter and the second regulating valve are electrically connected with the DCS control system, and the second regulating valve is used for according to DCS control system
On the inlet amount of hydrogen that is calculated adjust itself aperture, to control the inlet amount of hydrogen, second flowmeter is for measuring
It is passed into the amount of the intracorporal hydrogen of furnace；
The air feed component includes air feed pipeline, third flowmeter, third regulating valve, the air feed pipe
The connection of the burner of line and furnace body, the third flowmeter and the third regulating valve are set on the air feed pipeline, and
Third regulating valve and second flowmeter are electrically connected with the DCS control system, and third regulating valve is used for according to DCS control system
The inlet amount for the air being calculated adjusts itself aperture, and to control the inlet amount of air, third flowmeter has led to for measuring
Enter the amount to the air in hydrolysis furnace.
Preferably, the temperature measurer uses Dual-wavelength infrared thermometer, the temperature threshold set in the DCS control system
It is 1800 DEG C.
Preferably, the pressure control unit includes pressure transmitter, frequency converter, blower,
The pressure transmitter is set in the furnace tube of the furnace body, and is electrically connected with the DCS control system, for detecting
Pressure in furnace tube, and the pressure information in the furnace tube that will test is transferred to DCS control system；
Pressure threshold is additionally provided in the DCS control system, DCS control system is for detecting the pressure transmitter
The furnace tube in pressure information be compared with the pressure threshold, and according to pressure comparison result output pressure increase/
Attenuated signal；
The blower is connect with the outlet of the lower part of the furnace tube of the furnace body, for making furnace to furnace tube exhausting from inside to outside
Tiny structure is kept in cylinder；
The frequency converter is electrically connected with the blower, and is electrically connected with the DCS control system, is received for basis
The pressure increase/attenuated signal adjustment blower working power frequency, to adjust the revolving speed of blower.
Preferably, the hydrolysis furnace further includes tail gas control unit, and the tail gas control unit includes tails assay component
With mend hydrogen component,
The tails assay component is connect with the furnace tube of the furnace body, for the gas component in detection and analysis furnace tube,
And transmit the gas component information in detected furnace tube；
The benefit hydrogen component is connect with the furnace tube of the furnace body, is also connect with the tails assay component, for according to tail
Gas component information in the furnace tube that gas analytic unit detects is passed through hydrogen make-up into furnace tube.
Preferably, the tails assay component includes first gas analyzer,
The first gas analyzer is set to the top of the furnace tube, and is electrically connected with the DCS control system, for examining
The oxygen content on furnace tube top is surveyed, and the oxygen content information on the furnace tube top that will test is transferred to DCS control system；
The first oxygen content threshold value is additionally provided in the DCS control system, DCS control system is also used to first gas
The oxygen content information on the furnace tube top that body analyzer detects is compared with the first oxygen content threshold value, and is counted
The inlet amount of hydrogen make-up is calculated, then transmits the inlet amount information of hydrogen make-up；
The inlet amount information that hydrogen component is mended for the hydrogen make-up that basis receives hydrogen make-up into furnace tube.
Preferably, the tails assay component further includes second gas analyzer,
The second gas analyzer is set to the lower part of the furnace tube, and connect with the DCS control system, for detecting
The content of the oxygen of furnace tube lower part, hydrogen, and the oxygen content information for the furnace tube lower part that will test, hydrogen content information are transmitted
To DCS control system；
The second oxygen content threshold value and hydrogen content threshold value are additionally provided in the DCS control system, DCS control system is also used
Oxygen content information and the second oxygen content threshold in the furnace tube lower part for detecting the second gas analyzer
Value is compared, contains the hydrogen content information for the furnace tube lower part that the second gas analyzer detects with the hydrogen
Amount threshold value is compared, and the signal of increase/reduction hydrogen make-up inlet amount is exported according to comparison result；
It is described mend hydrogen component be also used to according to the DCS control system export the increase/reduction hydrogen make-up into
The inlet amount of the Signal Regulation hydrogen make-up of doses.
Preferably, the first gas analyzer, the second gas analyzer are all made of Zirconium oxide analyzer.
Preferably, the benefit hydrogen component includes hydrogen make pipeline, the 4th regulating valve, the 4th flowmeter,
The hydrogen make pipeline is connect with the middle part of the furnace tube, for being passed through hydrogen make-up into furnace tube；
4th regulating valve is set on the hydrogen make pipeline, and is connect with the DCS control system, and basis is used for
The inlet amount information of the hydrogen make-up received, and/or, the signal of the increase/reduction hydrogen make-up inlet amount is adjusted
Itself aperture is saved, to control the inlet amount of hydrogen make-up；
4th flowmeter is set on the hydrogen make pipeline, for measuring the supplement being passed into the furnace tube
The amount of hydrogen.
According to an aspect of the present invention, a kind of system for producing fumed silica is provided, including at deacidification furnace, tail gas
Device is managed, further includes the hydrolysis furnace of above-described production fumed silica, the outlet of the hydrolysis furnace and the deacidification furnace
Connection.
The hydrolysis furnace and system of production fumed silica provided by the invention, may be implemented pair by temperature control unit
The temperature of hydrolysis furnace flame is precisely controlled, and flame temperature is made to maintain optimal 1800 DEG C, by pressure control unit,
Make to hydrolyze and maintain suitable tiny structure in furnace, keeps residence time of the fumed silica generated in flame shorter, to obtain
Partial size is small, fumed silica product of large specific surface area；Pass through tail gas control unit, it is possible to reduce the production of chlorine in tail gas
It is raw, to reduce vent gas treatment difficulty, reduce the usage amount in subsequent vent gas treatment process to lye, hydrogen peroxide, correspondingly
Also the generation for just reducing sodium hypochlorite improves the fortune of the hydrolysis furnace in fumed silica production process and production system
Row safety can be realized the optimal combustion control of fumed silica hydrolysis furnace.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that the hydrolysis furnace of fumed silica is produced in embodiment 1；
Fig. 2 is in embodiment 1 to the control flow schematic diagram of hydrolysis in-furnace temperature；
Fig. 3 is in embodiment 1 to the control flow schematic diagram of hydrolysis furnace pressure；
Fig. 4 is in embodiment 1 to the control flow schematic diagram of hydrolysis furnace inner exhaust gas component.
In figure: 1- furnace body；11- burner；12- furnace tube；13- visor；14-DCS control system；2- temperature measurer；Tetra- chlorination of 3-
Silicon feeding line；31- first flowmeter；The first regulating valve of 32-；4- hydrogen feed line；41- second flowmeter；42- second is adjusted
Save valve；5- air feed pipeline；51- third flowmeter；52- third regulating valve；6- hydrogen make pipeline；61- stop valve；62-
4th flowmeter；The 4th regulating valve of 63-；71- first gas analyzer；72- second gas analyzer；8- pressure transmitter；9-
Frequency converter；10- blower.
Specific embodiment
Technical solution in order to enable those skilled in the art to better understand the present invention, below in conjunction with attached in the present invention
Figure, carries out clear, complete description to the technical solution in the present invention, it is clear that described embodiment is one of the invention
Point embodiment, rather than whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making wound
Every other embodiment obtained under the premise of the property made is worked, belongs to protection scope of the present invention.
Embodiment 1
The present embodiment discloses a kind of hydrolysis furnace for producing fumed silica, is used for gaseous silicon (hereinafter referred to as
Silicon tetrachloride) it is that production fumed silica is hydrolyzed in raw material in thermal-flame.The hydrolysis furnace mainly includes furnace body 1, DCS
Control system 14 (i.e. dcs Distributed Control System), temperature control unit, pressure control
Unit, furnace body 1 include burner 11 and furnace tube 12, and DCS control system is for centralized control and coordinates temperature control unit, pressure control
Unit and exhaust gas composition control unit processed, specific as follows:
(1) temperature control unit
Temperature control unit includes temperature measurer 2, feeding mechanism, and temperature measurer 2 is set on the furnace body 1 of hydrolysis furnace, is also controlled with DCS
System 14 processed is electrically connected, the temperature of the flame generated in the furnace body 1 for detecting hydrolysis furnace, the temperature that is denoted as T, and will test
Information is transferred to DCS control system 14；It is equipped with temperature threshold in DCS control system 14, is denoted as T0, DCS control system 14 is used for
Fixed temperature threshold T is pushed up by setting in temperature information that temperature measurer 2 detects and DCS control system 140It is compared, further according to temperature
Degree comparison result calculates the inlet amount of silicon tetrachloride, hydrogen, air, and transmits these calculated inlet amount information and (count
The inlet amount information of the silicon tetrachloride of calculating, hydrogen, air)；Feeding mechanism is connect with the furnace body 1 of hydrolysis furnace, is also controlled with DCS
System 14 is electrically connected, for according to the inlet amount for passing out silicon tetrachloride, hydrogen, air by DCS control system 14 received
Information is passed through silicon tetrachloride, hydrogen and air into the furnace body 1 of hydrolysis furnace.
Further, feeding mechanism includes that silicon tetrachloride feeding component, hydrogen feeding assembly, air feed component are (main
The oxygen being to provide in air), in which:
Silicon tetrachloride feeding component is connect with the burner 11 of the furnace body 1 of hydrolysis furnace, is also electrically connected with DCS control system 14,
The inlet amount that silicon tetrachloride is additionally provided in DCS control system (is denoted as FT1, gone out according to the Production rate of setting or plan), tetrachloro
SiClx feeding assembly is used for the inlet amount FT according to the silicon tetrachloride set in the DSC control system 14 received1To hydrolysis furnace
Furnace body 1 burner 11 in be passed through silicon tetrachloride, and silicon tetrachloride feeding information is fed back into DCS control system 14.
Specifically, silicon tetrachloride feeding component includes silicon tetrachloride feeding pipeline 3, first flowmeter 31, the first regulating valve
32, silicon tetrachloride feeding pipeline 3 is connect with the burner 11 of the furnace body 1 of hydrolysis furnace, and first flowmeter 31 and the first regulating valve 32 are
On silicon tetrachloride feeding pipeline 3, and first flowmeter 31 and the first regulating valve 32 are electrically connected with DCS control system 14,
First flowmeter 31 and the first regulating valve 32 composition silicon tetrachloride flow indicate control loop, are denoted as FIC1, for being controlled according to DCS
The inlet amount of the silicon tetrachloride set in system processed 14 is passed through silicon tetrachloride to the burner 11 of the furnace body 1 of hydrolysis furnace, and by tetrachloro
The charging information of SiClx feeds back to DCS control system 14, wherein the first regulating valve 32 is used for according to setting in DCS control system 14
The inlet amount FT of fixed silicon tetrachloride1Itself aperture is adjusted, to control the inlet amount of silicon tetrachloride；First flowmeter 31 is for surveying
Amount has been passed into the amount of the silicon tetrachloride in the burner 11 of the furnace body 1 of hydrolysis furnace.
Hydrogen feeding assembly is connect with the burner 11 of the furnace body 1 of hydrolysis furnace, is also electrically connected with DCS control system 14, in DCS
The charge ratio that hydrogen and silicon tetrachloride are additionally provided in control system 14 (is denoted as K1, obtained according to material reaction EQUILIBRIUM CALCULATION FOR PROCESS), DCS
Control system 14 is according to the inlet amount FT of silicon tetrachloride1, hydrogen and silicon tetrachloride charge ratio K1, calculate the inlet amount of hydrogen
(it is denoted as FT2, FT2=FT1*K1), the inlet amount for the hydrogen that hydrogen feeding assembly is used to be calculated according to DCS control system 14
FT2It is passed through hydrogen into the burner 11 of the furnace body 1 of hydrolysis furnace, and hydrogen charging information is fed back into DCS control system 14.
Specifically, hydrogen feeding assembly includes hydrogen feed line 4, second flowmeter 41, the second regulating valve 42, hydrogen into
Expects pipe line 4 is connect with the burner 11 of the furnace body 1 of hydrolysis furnace, and second flowmeter 41 and the second regulating valve 42 are set to hydrogen feed tube
On line 4, and second flowmeter 41 and the second regulating valve 42 are electrically connected with DCS control system 14, second flowmeter 41 and second
Regulating valve 42 forms hydrogen flowing quantity and indicates control loop, is denoted as FIC2, hydrogen for being calculated according to DCS control system 14
Inlet amount FT2It is passed through hydrogen into the burner 11 of the furnace body 1 of hydrolysis furnace, and the charging information of hydrogen is fed back into DCS control
System 14, wherein the inlet amount FT for the hydrogen that the second regulating valve 42 is used to be calculated according to DCS control system 142It adjusts certainly
Body aperture, to control the inlet amount of hydrogen；Second flowmeter 41, which is used to measure, to be passed into the burner 11 of the furnace body 1 of hydrolysis furnace
Hydrogen amount.
Air feed component is connect with the burner 11 of the furnace body 1 of hydrolysis furnace, is also electrically connected with DCS control system 14, in DCS
The charge ratio that air and hydrogen are additionally provided in control system 14 (is denoted as K2, obtained according to material reaction EQUILIBRIUM CALCULATION FOR PROCESS), DCS control
System 14 is according to the inlet amount FT of hydrogen2, air and hydrogen charge ratio K2, the inlet amount for calculating air (is denoted as FT3, FT3
=FT2*K2), the inlet amount FT for the air that air feed component is used to be calculated according to DCS control system 143To hydrolysis furnace
It is passed through air in burner 11, and air feed information is fed back into DCS control system 14.
Specifically, air feed component includes air feed pipeline 5, third flowmeter 51, third regulating valve 52, air into
Expects pipe line 5 is connect with the burner 11 of the furnace body 1 of hydrolysis furnace, and third flowmeter 51 and third regulating valve 52 are set to air feed pipe
On line 5, and third flowmeter 51 and third regulating valve 52 are electrically connected with DCS control system 14, third flowmeter 51 and third
Regulating valve 52 forms air mass flow and indicates control loop, is denoted as FIC3, air for being calculated according to DCS control system 14
Inlet amount FT3It is passed through air into the burner 11 of the furnace body 1 of hydrolysis furnace, and the charging information of air is fed back into DCS control
System 14, wherein the inlet amount FT for the air that third regulating valve 52 is used to be calculated according to DCS control system 143It adjusts certainly
Body aperture, to control the inlet amount of air；Third flowmeter 51, which is used to measure, to be passed into the burner 11 of the furnace body 1 of hydrolysis furnace
Air amount.
Further, the first flowmeter 31 in the present embodiment, second flowmeter 41, the type of third flowmeter 51 can roots
It is determined according to actual conditions, can be volume flowmeter, be also possible to mass flowmenter, the present embodiment is not further qualified.
Specifically, temperature measurer 2 is set on 13 channel of visor of the burner 11 of the furnace body 1 of hydrolysis furnace, for detecting hydrolysis furnace
Furnace body 1 burner 11 in hydrogen and oxygen react generation flame temperature, and the temperature T for the flame that will test
Information is transferred to DCS control system 14.In the present embodiment, temperature measurer 2 is preferably using can issue infrared waves, ultraviolet light wave
Dual-wavelength infrared thermometer.
Temperature measurer 2 is also connect with DCS control system 14, and temperature threshold T is also set in DCS control system 140.This reality
Apply the temperature threshold T in example0Preferably 1800 DEG C, because of it is discovered by experiment that the fumed silica produced at 1800 DEG C
Partial size is small, large specific surface area, i.e., the better quality of resulting fumed silica.
DSC control system 14 controls the temperature T information of the flame generated in burner 11 that temperature measurer 2 detects and DCS
The temperature threshold T set in system 140It is compared, and silicon tetrachloride, hydrogen, air is adjusted according to temperature comparison result and matched
Than the i.e. charge ratio K according to temperature comparison result to the hydrogen and silicon tetrachloride that have been set in DCS control system1, air and hydrogen
The charge ratio K of gas2It is revised, further according to the charge ratio K of revised hydrogen and silicon tetrachloride1, air and hydrogen charge ratio
K2Calculate separately out the inlet amount of revised hydrogen, the inlet amount of air, and by the inlet amount information of revised hydrogen, sky
The inlet amount information of gas is transferred to hydrogen feeding assembly, air feed component respectively, makes hydrogen feeding assembly according to revised
The inlet amount of hydrogen is passed through hydrogen into the burner 11 of the furnace body 1 of hydrolysis furnace, makes air feed component according to revised air
Inlet amount be passed through air into the burner 11 of the furnace body 1 of hydrolysis furnace, to realize to the temperature regulation and control of flame.
The tune of the temperature of the flame generated in the burner 11 of the furnace body 1 of 14 pairs of hydrolysis furnaces of DCS control system in the present embodiment
Section and control mode make according to temperature comparison result adjust silicon tetrachloride, hydrogen, air proportion realize, specific tetrachloro
SiClx, the regulative mode of the proportion of hydrogen, air are preferred are as follows: keep the charging of silicon tetrachloride not change, when temperature measurer 2 detects
Burner 11 in generate flame temperature T be greater than DCS control system 14 in set temperature threshold T0When (1800 DEG C), DCS
Control system is according to comparison temperature as a result, by the charge ratio K of hydrogen and silicon tetrachloride1, air and hydrogen charge ratio K2It is fitted
When reduction (specifically reducing how many specific algorithms, the present embodiment is not further qualified), subtract the inlet amount of hydrogen and air
It is few, so that the temperature for making hydrogen and oxygen react the flame generated reduces；When the fire generated in the burner 11 that temperature measurer 2 detects
The temperature T of flame is less than the temperature threshold T set in DCS control system 140When, DCS control system, will according to temperature comparison result
The charge ratio K of hydrogen and silicon tetrachloride1, air and hydrogen charge ratio K2Suitably increased (specifically increase how many algorithms,
The present embodiment is not further qualified), increase the inlet amount of hydrogen and air, to make hydrogen and oxygen reaction in burner 11
The temperature of the flame of generation increases.
As shown in Fig. 2, the hydrolysis furnace of the production fumed silica in the present embodiment is by temperature control unit to hydrolysis
The temperature controlled processes of flame in furnace are as follows:
S101 sets the inlet amount FT of silicon tetrachloride in DCS control system 141, hydrogen and silicon tetrachloride charge ratio
K1, air and hydrogen charge ratio K2And temperature threshold T0；
S102, DCS control system 14 calculates the inlet amount FT of initial hydrogen2, air charging FT3, and transmit tetrachloro
Inlet amount information, the inlet amount information of hydrogen, the inlet amount information of air of SiClx；
S103, silicon tetrachloride feeding pipeline 3, hydrogen feed line 4, air feed pipeline 5 are respectively according to four received
The inlet amount information of silicon chloride, the inlet amount information of hydrogen, the inlet amount information of air are into the burner 11 of the furnace body 1 of hydrolysis furnace
It is passed through silicon tetrachloride, hydrogen, air, the first reaction in the burner 11 of hydrolysis furnace of the oxygen in hydrogen and air is made to generate water, and
Flame is issued, reaction is hydrolyzed in flame and generates fumed silica for silicon tetrachloride；
S104, using Dual-wavelength infrared thermometer to the temperature of flame generated in the burner 11 of the furnace body 1 of hydrolysis furnace into
Row detection, and the temperature T information for the flame that will test is transferred to DCS control system 14；
The temperature that S105, DCS control system 14 will be set in the temperature T information of the flame received and DCS control system 14
Spend threshold value T0It is compared, judges whether the temperature T of the flame detected is more than temperature threshold T0, and according to temperature comparison result
To the charge ratio K of hydrogen and silicon tetrachloride1, air and hydrogen charge ratio K2It is revised, in which:
Work as T > T0, then step S106 is carried out；
As T < T0, then step S108 is carried out；
Work as T=T0, then continue to be fed by the inlet amount in step S103, until charging terminates.
S106 reduces the charge ratio K of hydrogen and silicon tetrachloride1, reduce the charge ratio K of air and hydrogen2, and according to revision
K afterwards1、K2Calculate the inlet amount of hydrogen, the inlet amount of air, and by calculated result be transferred to hydrogen feeding assembly, air into
Expect component, and is transferred to step S107；
S107 reduces the inlet amount of the aperture regulation hydrogen of the second regulating valve 42, reduces the aperture tune of third regulating valve 52
The inlet amount of air is saved, and is transferred to step S104；
S108 increases the charge ratio K of hydrogen and silicon tetrachloride1, increase the charge ratio K of air and hydrogen2, and according to revision
K afterwards1、K2The inlet amount of hydrogen, the inlet amount of air are calculated, and enters step S109；
S109 increases the inlet amount of the aperture regulation hydrogen of the second regulating valve 42, increases the aperture tune of third regulating valve 52
The inlet amount of air is saved, and enters step S104.
The hydrolysis furnace of production fumed silica in the present embodiment, by the way that temperature control unit is arranged, by silicon tetrachloride
Feeding assembly, hydrogen feeding assembly, air feed component respectively gradually adjust the inlet amount of silicon tetrachloride, hydrogen, air
Section, progressivelyes reach the temperature (1800 DEG C of temperature threshold for reaching setting) of optimal flame, and, control simple with structure is precisely
The advantages that.
(2) pressure control unit
Pressure control unit is connect with the furnace tube 12 of furnace body 1, and is electrically connected with DCS control system 14, for adjusting furnace body 1
Interior pressure, to control residence time of the fumed silica generated in flame.
Specifically, pressure control unit includes pressure transmitter 8,9 (i.e. Variable-frequency of frequency converter
Drive, VFD control the electric control appliance of ac motor by changing motor frequency mode of working power supply), blower 10,
Wherein:
Pressure transmitter 8 is set in the furnace tube 12 of furnace body 1, and is electrically connected with DCS control system 14, for detecting furnace body 1
Furnace tube 12 in pressure, the pressure information in furnace tube 12 that is denoted as P, and will test is transferred to DCS control system；In DCS
It is additionally provided with pressure threshold in control system 14, is denoted as P0, furnace tube of the DCS control system 14 for detecting pressure transmitter 8
The pressure threshold P set in pressure P and DCS control system 14 in 120It is compared, and is exported and pressed according to pressure comparison result
Power increase/attenuated signal.
Further, the pressure in the furnace tube 12 in the hydrolysis furnace in the present embodiment needs to be maintained tiny structure, tiny structure
Size set and adjusted according to practical condition, the tiny structure of general actual set is -3kPa~-5kPa,
It is not further qualified, is preferably -3kPa in the present embodiment.
Blower 10 is connect with the outlet of the furnace tube 12 of furnace body 1, and the outlet of furnace tube 12 is preferably disposed to the lower part of furnace tube 12, be used for
To the exhausting from inside to outside of furnace tube 12 of hydrolysis furnace, makes to hydrolyze and keep tiny structure in the furnace tube of furnace.
Frequency converter 9 is electrically connected with the input power of blower 10, and frequency converter 9 is also electrically connected with DCS control system 14, is used for root
The pressure increase exported according to the DCS control system 14 received /attenuated signal adjustment blower 10 working power frequency, to adjust
The revolving speed of blower 10 controls the pressure in the furnace tube 12 of furnace body 1 in suitable tiny structure.
In the present embodiment, by the furnace bodies 1 of 10 pairs of hydrolysis furnaces of blower exhausting from inside to outside, make to protect in the furnace tube 12 of furnace body 1
Tiny structure is held, one suction is formed to the burner 11 of hydrolysis furnace, makes the flame generated in burner quickly down (i.e. to furnace tube 12
Lower part) movement, make shorter residence time of the fumed silica in flame generated, thus make fumed silica keep compared with
Small partial size and biggish specific surface area.
As shown in figure 3, the hydrolysis furnace for producing fumed silica in the present embodiment passes through pressure control unit to hydrolysis furnace
Interior pressure control procedure is as follows:
Pressure threshold P is arranged in S201 in DCS control system 140；
S202 starts blower, to the exhausting from inside to outside of furnace tube 12 of hydrolysis furnace；
S203, the pressure P that the pressure in the furnace tube 12 of furnace body 1 is detected, and will test using pressure transmitter 8
Information is transferred to DCS control system 14；
S204, DCS control system 14 will receive the pressure threshold P set in pressure P and DCS control system 140It carries out
Compare, judges whether the pressure P in furnace tube is more than pressure threshold P0, in which:
Work as P > P0, then step S205 is carried out；
As P < P0, then step S206 is carried out；
Work as P=P0, then continue to carry out exhausting from inside to outside to furnace tube by step S202, until production process terminates.
The working power frequency of blower 10 is tuned up by frequency converter 9, to make 10 faster rotational speed of blower, is gone forward side by side by S205
Enter step S202；
The working power frequency of blower 10 is turned down by frequency converter 9, to make 10 spin down of blower, is gone forward side by side by S206
Enter step S202；
The present embodiment can make water by the way that the pressure in the frequency and furnace tube of the working power of blower is carried out interlocked control
The pressure solved in the furnace tube of furnace maintains suitable tiny structure, such as -3kPa (pressure threshold set), to guarantee to fire in material
Burning makes the fumed silica of generation residence time in flame shorter under the premise of stablizing, to obtain, partial size is small, compares table
The big product of area.
In the actual production process, the hydrolyzing silicon tetrachloride reaction in the burner 11 in order to make to hydrolyze furnace is more abundant, needs
Keep the oxygen for hydrolyzing the burner 11 of furnace excessive, and excessive oxygen can produce chlorine with the hcl reaction of production in tail gas, because
This, needs to handle oxygen excessive in tail gas, to reduce the generation of chlorine.
Further, the hydrolysis furnace of the production fumed silica in the present embodiment further includes tail gas control unit.
(3) tail gas control unit
Tail gas control unit includes tails assay component and benefit hydrogen component, in which: the furnace tube of tails assay component and furnace body 1
12 connections for the gas component in detection and analysis furnace tube 12, and transmit the gas component letter in detected furnace tube 12
Breath；It mends hydrogen component to connect with the furnace tube 12 of furnace body 1, also be connect with tails assay component, for according to tails assay component detection
To furnace tube 12 in gas component information be passed through hydrogen make-up into the furnace tube 12 of furnace body 1.
Specifically, tails assay component is connect with the furnace tube 12 of furnace body 1, in the furnace tube 12 of detection and analysis furnace body 1
Gas component, tails assay component is also electrically connected with DCS control system 14, is also used to transmit the furnace of detected furnace body 1
Gas component information in cylinder 12；The first oxygen content threshold value W is additionally provided in DCS control system 1410(the i.e. top of furnace tube 12
Oxygen content threshold value, be denoted as W10, in the present embodiment, W10Preferably 8%), DCS control system 14 is also used to tails assay
Component detection to furnace tube 12 in the first oxygen content threshold value W for setting in gas component information and DCS control system 1410It carries out
Compare, the inlet amount of hydrogen make-up required for calculating further according to comparison result (is denoted as FT4), and transmit calculated supplement
The inlet amount information of hydrogen；It mends hydrogen component to connect with the furnace tube 12 of furnace body 1, preferably be connect with the middle part of furnace tube 12, and also and DCS
Control system 14 is electrically connected, for according to the inlet amount information of the calculated hydrogen make-up of DCS control system 14 received from
The middle part of furnace tube 12 is passed through hydrogen make-up into the furnace tube 12 of furnace body 1, makes the oxygen in the tail gas in the hydrogen and furnace tube 12 of supplement
Gas reacts, and consumes excessive oxygen, the chance that the chlorine reaction in oxygen and tail gas generates chlorine is reduced, to control furnace
Exhaust gas composition in cylinder, to reduce vent gas treatment difficulty.
Further, tails assay component includes first gas analyzer 71, and first gas analyzer 71 is set to furnace tube 12
Top, and be electrically connected with DCS control system 14, the oxygen content on the top for detecting furnace tube 12 (i.e. the first oxygen content,
It is denoted as W1), and the oxygen content information on the top for the furnace tube 12 that will test is transferred to DCS control system 14, DCS control system
Oxygen content information (the i.e. first oxygen content W on the top of 14 furnace tubes 12 for detecting first gas analyzer 711) and DCS
The the first oxygen content threshold value W set in control system 1410Be compared, further according to comparison result calculate hydrogen make-up into
Doses FT4, and transmit the inlet amount information of calculated hydrogen make-up.
Further, tails assay component further includes second gas analyzer 72, and second gas analyzer 72 is set to furnace tube
12 lower part, and be electrically connected in DCS control system 14, the content of the oxygen of the lower part for detecting furnace tube 12, hydrogen, and will inspection
Oxygen content information (i.e. the second oxygen content W of the lower part of the furnace tube 12 measured2), hydrogen content information be transferred to DCS control
System 14；The second oxygen content threshold value is additionally provided in DCS control system 14, and (i.e. the oxygen of the lower part of the furnace tube 12 of hydrolysis furnace contains
Threshold value is measured, W is denoted as20, in the present embodiment, W20Preferably 2%) and hydrogen content threshold value W30(the i.e. lower part of the furnace tube 12 of hydrolysis furnace
Hydrogen content threshold value, be denoted as W30, in the present embodiment, preferably 1%-2%), DCS control system 14 is also used to second gas
(i.e. the first oxygen content, is denoted as W to the oxygen content information of the lower part of the furnace tube 12 for the hydrolysis furnace that analyzer 72 detects1) with
The the second oxygen content threshold value W set in DCS control system 1420The water for being compared, detecting second gas analyzer 72
Solve the hydrogen content threshold value W set in the hydrogen content information and DCS control system 14 of the lower part of the furnace tube 12 of furnace30Compared
Compared with, and according to the signal of comparison result output increase/reduction hydrogen make-up inlet amount.
Further, the first gas analyzer 71 in the present embodiment, second gas analyzer 72 are all made of zirconium oxide point
Analyzer, Zirconium oxide analyzer can analyze two kinds of oxygen, hydrogen gas components simultaneously, it can while detecting oxygen and hydrogen
Content.
Further, mending hydrogen component includes hydrogen make pipeline 6, stop valve 61, the 4th flowmeter 62, the 4th regulating valve
63, in which: hydrogen make pipeline 6 is connect with the middle part of the furnace tube 12 of hydrolysis furnace, for being passed through benefit into the furnace tube 12 of hydrolysis furnace
It is flushed with hydrogen gas；Stop valve 61 is set on hydrogen make pipeline 6, and be electrically connected with DCS control system 14, for basis receive by
The inlet amount information of hydrogen make-up that DCS control system 14 exports, increase/reduction hydrogen make-up inlet amount signal, open or
Close hydrogen make pipeline 6；4th flowmeter 62 and the 4th regulating valve 63 composition hydrogen make-up flow indicate control loop, are denoted as
FIC4, the 4th regulating valve 63 is set on hydrogen make pipeline 6, for according to the benefit transmitted by DCS control system 14 received
It is flushed with hydrogen the inlet amount information of gas, and/or, the signal of increase/reduction hydrogen make-up inlet amount is exported, the 4th regulating valve 63 is adjusted
The aperture of itself, to control the inlet amount of hydrogen make-up；4th flowmeter 62 is set on hydrogen make pipeline 6, for measuring
It is passed into the inlet amount of the hydrogen make-up in the furnace tube 12 of hydrolysis furnace.The type of the 4th flowmeter 62 in the present embodiment can basis
Actual conditions determine, are not further qualified.
As shown in figure 4, the hydrolysis furnace of the production fumed silica in this example is by tail gas control unit to hydrolysis furnace
Interior exhaust gas composition control process is as follows:
S301 sets the first oxygen content threshold value W in DCS control system 1410(in the present embodiment, the first oxygen content
Threshold value W10It is 8%, that is to say, that 8%) the oxygen content threshold value for hydrolyzing the top of the furnace tube of furnace is, sets the second oxygen content
Threshold value W20(in the present embodiment, the second oxygen content threshold value W20It is 2%, that is to say, that hydrolyze the oxygen of the lower part of the furnace tube of furnace
2%) content threshold value is, sets hydrogen content threshold value W30For 1% (in the present embodiment, hydrogen content threshold value W30It is 1%, that is,
It says, hydrolyzes the hydrogen content threshold value W of the lower part of the furnace tube 12 of furnace30For 1%)；
S302, using the Zirconium oxide analyzer (i.e. first gas analyzer 71) on the top for being set to furnace tube 12 to furnace tube 12
Oxygen content in the tail gas on top carries out real-time online detection, and the oxygen in the tail gas on the top for the furnace tube 12 that will test
(i.e. the first oxygen content, is denoted as W to content1) information is transferred to DCS control system 14；
The first oxygen content W that S303, DCS control system 14 will test1With set in DCS control system 14 first
Oxygen content threshold value W10It is compared, judges the first oxygen content W1Whether more than the first oxygen content threshold value W10, in which:
W1> W10, then step S304 is carried out；
W1≤W10, then continue step S302, until production process terminates.
S304, DCS control system calculate the inlet amount of hydrogen make-up, and transmit the inlet amount information for calculating hydrogen make-up
To benefit hydrogen component, and it is transferred to step 305；
S305 opens stop valve 61 and the 4th regulating valve 63, hydrogen make-up is passed through into furnace tube, and enter step S306；
S306, using the Zirconium oxide analyzer (i.e. second gas analyzer 72) for the lower part for being set to furnace tube 12 to furnace tube 12
The content of the oxygen in tail gas, hydrogen after the deoxygenation of lower part carries out real-time online detection, and under the furnace tube 12 that will test
Oxygen content (i.e. the second oxygen content W in the tail gas after deoxygenation in portion2) information, hydrogen content (be denoted as W3) information
It is transferred to DCS control system 14；
The second oxygen content W that S307, DCS control system 14 will test2With set in DCS control system 14 second
Oxygen content threshold value W20It is compared, judges the second oxygen content W2Whether more than the second oxygen content threshold value W20, judge hydrogen
Content W3It whether is more than hydrogen content threshold value W30, wherein:
Work as W2> W20,W3< W30Then carry out step S308；
Work as W2≤W20, and W3> W30, then step S309 is carried out；
Work as W3≤W30, and W2≤W20, then continue step S306, until production process terminates.
S308, increase the 4th regulating valve 63 aperture, with increase hydrogen make-up inlet amount (but cannot beyond hydrogen it is quick-fried
Fried limit range), and enter step S306；
S309 reduces the aperture of the 4th regulating valve 63 or closes stop valve 61 and gone forward side by side with reducing the inlet amount of hydrogen make-up
Enter step S306.
The present embodiment by the way that the inlet amount of hydrogen make-up and oxygen content, the hydrogen content in furnace tube 12 are interlocked,
Change the inlet amount of hydrogen make-up in real time according to oxygen content information, the hydrogen content information in furnace tube 12.When the first oxygen contains
When amount is higher than the first oxygen threshold value, the inlet amount of hydrogen make-up is increased, hydrogen and oxygen is made to react reduction hydrolysis as much as possible
The oxygen content in tail gas in furnace furnace tube 12, until when in the tail gas after deoxygenation of the lower part of the furnace tube 12 detected
Oxygen reaches control and requires (to be no more than the second oxygen content threshold value W20)；Second oxygen content is lower than the second oxygen content threshold value
When, reduce the inlet amount of hydrogen make-up, to avoid causing hydrogen to waste；When hydrogen content is higher than hydrogen content threshold value, explanation
It is excessive to fill the hydrogen make-up that the middle part of furnace tube 12 is passed through, closes stop valve 61 immediately, stops hydrogen make-up.
DCS control system in the present embodiment can be controlled in Zhejiang using the ECS700 system controlled in Zhejiang
Temperature threshold T can be set in ECS700 system (DCS control system)0, pressure threshold P0, the first oxygen content threshold value W10,
Two oxygen content threshold value W20, hydrogen content threshold value W30Deng all the above control function may be implemented.
Further, in the present embodiment, temperature threshold T0Preferably 1800 DEG C；Pressure threshold P0Preferably -3kPa~-
5kPa, more preferably -3kPa；First oxygen content threshold value W10Preferably 8%；Second oxygen content threshold value W20Preferably 2%；
Hydrogen content threshold value W30Preferably 1%-2%, more preferably 2%.
A kind of system for producing fumed silica, including above-described production gas phase titanium dioxide is also disclosed in the present embodiment
The hydrolysis furnace and deacidification furnace and exhaust gas processing device (process) of silicon.
Specifically, the blower being arranged in deacidification furnace entrance and the outlet of hydrolysis furnace is connect, the gas for being come out to hydrolysis furnace
The mixed gas such as aerosil carry out depickling and obtain the gas phase two of high-purity to remove the sour gas such as hydrogen chloride therein
Silica product；The offgas outlet of vent gas treatment process and deacidification furnace connection, for carrying out vent gas treatment, to reduce pernicious gas
Discharge, avoid pollution environment.
The system of production fumed silica in the present embodiment, when carrying out fumed silica production, firstly, hydrogen
The burning of burner 11 with oxygen in hydrolysis furnace generates water, and releases flame；Then, burner of the gaseous silicon in hydrolysis furnace
Production fumed silica is hydrolyzed in thermal-flame in 11 and hydrogen chloride, the fumed silica of production are gradually hydrolyzing
The furnace tube 12 of furnace is assembled, and aggregation is formed, finally, being taken off from the output of outlet blower 10 to the deacidification furnace of the furnace tube 12 of hydrolysis furnace
Acid processing (mainly removes de-chlorine hydride), and the fumed silica of high-purity can be obtained.The tail gas for obtaining deacidification furnace enters tail
Gas disposal process (device), is discharged after vent gas treatment.
The present embodiment is disclosed for producing the hydrolysis furnace of fumed silica, may be implemented pair by temperature control unit
The temperature of hydrolysis furnace flame is precisely controlled, and flame temperature is made to maintain optimal 1800 DEG C, by pressure control unit,
Make to hydrolyze the tiny structure for maintaining suitable -3KPa in furnace, keep residence time of the fumed silica generated in flame shorter,
To obtain, partial size is small, fumed silica product of large specific surface area；Pass through tail gas control unit, it is possible to reduce chlorine in tail gas
The generation of gas reduces the usage amount in subsequent vent gas treatment process to lye, hydrogen peroxide to reduce vent gas treatment difficulty,
The generation for correspondingly also just reducing sodium hypochlorite improves hydrolysis furnace and system fortune in fumed silica production process
Row safety can be realized the optimal combustion control of fumed silica hydrolysis furnace.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from
In the case where mind and essence, various changes and modifications can be made therein, these variations and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of hydrolysis furnace for producing fumed silica, including furnace body (1), which is characterized in that further include DCS control system
(14), temperature control unit, pressure control unit,
The temperature control unit includes temperature measurer (2), feeding mechanism, and the temperature measurer is set on the furnace body (1), and with institute
DCS control system (14) electrical connection is stated, for detecting the temperature of the flame generated in furnace body, and the temperature information that will test passes
It is handed to DCS control system；Temperature threshold is equipped in the DCS control system, what DCS control system was used to detect temperature measurer
Temperature information is compared with the temperature threshold, and calculates the inlet amount of silicon tetrachloride, hydrogen, air, then transmit these
Inlet amount information；The feeding mechanism is connect with the furnace body (1), is also electrically connected with the DCS control system (14), according to connecing
The inlet amount information that the DCS control system received passes out is passed through silicon tetrachloride, hydrogen and air into furnace body；
The pressure control unit is connect with the furnace tube (12) of the furnace body, and is electrically connected with the DCS control system (14), is used
In the intracorporal pressure of regulating stove, to control residence time of the fumed silica generated in flame.
2. the hydrolysis furnace of production fumed silica according to claim 1, which is characterized in that the feeding mechanism includes
Silicon tetrachloride feeding component, hydrogen feeding assembly, air feed component,
The silicon tetrachloride feeding component includes silicon tetrachloride feeding pipeline (3), first flowmeter (31), the first regulating valve
(32), the silicon tetrachloride feeding pipeline is connect with the burner (11) of the furnace body (1), the first flowmeter and described first
Regulating valve is set on silicon tetrachloride feeding pipeline, and first flowmeter and the first regulating valve with the DCS control system
(14) it being electrically connected, the first regulating valve is used to adjust itself aperture according to the inlet amount of the silicon tetrachloride set in DCS control system,
To control the inlet amount of silicon tetrachloride, first flowmeter is for measuring the amount for being passed into the intracorporal silicon tetrachloride of furnace；
The hydrogen feeding assembly includes hydrogen feed line (4), second flowmeter (41), the second regulating valve (42), the hydrogen
Gas feeding line is connect with the burner (11) of the furnace body (1), and the second flowmeter and second regulating valve are set to hydrogen
On gas feeding line, and second flowmeter and the second regulating valve are electrically connected with the DCS control system (14), the second regulating valve
For adjusting itself aperture according to the inlet amount for the hydrogen being calculated in DCS control system, to control the inlet amount of hydrogen, the
Two flowmeters are for measuring the amount for being passed into the intracorporal hydrogen of furnace；
The air feed component includes air feed pipeline (5), third flowmeter (51), third regulating valve (52), the sky
Gas feeding line is connect with the burner (11) of furnace body (1), and the third flowmeter and the third regulating valve are set to the sky
On gas feeding line, and third regulating valve and second flowmeter are electrically connected with the DCS control system (14), and third regulating valve is used
In adjusting itself aperture according to the inlet amount for the air being calculated in DCS control system, to control the inlet amount of air, third
Flowmeter is used to measure the amount for the air being passed into hydrolysis furnace.
3. the hydrolysis furnace of production fumed silica according to claim 1, which is characterized in that the temperature measurer (2) is adopted
With Dual-wavelength infrared thermometer, the interior temperature threshold set of the DCS control system (14) is 1800 DEG C.
4. the hydrolysis furnace of production fumed silica according to claim 1, which is characterized in that the pressure control unit
Including pressure transmitter (8), frequency converter (9), blower (10),
The pressure transmitter is set in the furnace tube (12) of the furnace body (1), and is electrically connected with the DCS control system (14),
For detecting the pressure in furnace tube, and the pressure information in the furnace tube that will test is transferred to DCS control system；
Pressure threshold is additionally provided in the DCS control system (14), DCS control system is for detecting the pressure transmitter
The furnace tube in pressure information be compared with the pressure threshold, and according to pressure comparison result output pressure increase/
Attenuated signal；
The blower is connect with the outlet of the lower part of the furnace tube (12) of the furnace body (1), for making to furnace tube exhausting from inside to outside
Tiny structure is kept in furnace tube；
The frequency converter is electrically connected with the blower (10), and is electrically connected with the DCS control system (14), for according to reception
The pressure increase arrived/attenuated signal adjustment blower working power frequency, to adjust the revolving speed of blower.
5. the hydrolysis furnace of production fumed silica according to claim 1, which is characterized in that the hydrolysis furnace further includes
Tail gas control unit, the tail gas control unit include tails assay component and mend hydrogen component,
The tails assay component is connect with the furnace tube (12) of the furnace body (1), for the gas group in detection and analysis furnace tube
Point, and transmit the gas component information in detected furnace tube；
The benefit hydrogen component is connect with the furnace tube (12) of the furnace body (1), is also connect with the tails assay component, and basis is used for
Tails assay component detection to furnace tube in gas component information hydrogen make-up is passed through into furnace tube.
6. the hydrolysis furnace of production fumed silica according to claim 5, which is characterized in that the tails assay component
Including first gas analyzer (71),
The first gas analyzer is set to the top of the furnace tube (12), and is electrically connected with the DCS control system (14), uses
Oxygen content in detection furnace tube top, and the oxygen content information on the furnace tube top that will test is transferred to DCS control system；
It is additionally provided with the first oxygen content threshold value in the DCS control system (14), DCS control system is also used to first gas
The oxygen content information on the furnace tube top that body analyzer detects is compared with the first oxygen content threshold value, and is counted
The inlet amount of hydrogen make-up is calculated, then transmits the inlet amount information of hydrogen make-up；
The inlet amount information that hydrogen component is mended for the hydrogen make-up that basis receives hydrogen make-up into furnace tube.
7. the hydrolysis furnace of production fumed silica according to claim 6, which is characterized in that the tails assay component
It further include second gas analyzer (72),
The second gas analyzer is set to the lower part of the furnace tube (12), and is electrically connected with the DCS control system (14), uses
In the content of the detection oxygen of furnace tube lower part, hydrogen, and the oxygen content information for the furnace tube lower part that will test, hydrogen content are believed
Breath is transferred to DCS control system；
It is additionally provided with the second oxygen content threshold value and hydrogen content threshold value in the DCS control system (14), DCS control system is also used
Oxygen content information and the second oxygen content threshold in the furnace tube lower part for detecting the second gas analyzer
Value is compared, contains the hydrogen content information for the furnace tube lower part that the second gas analyzer detects with the hydrogen
Amount threshold value is compared, and the signal of increase/reduction hydrogen make-up inlet amount is exported according to comparison result；
It is described mend hydrogen component be also used to according to the DCS control system (14) export the increase/reduction hydrogen make-up into
The inlet amount of the Signal Regulation hydrogen make-up of doses.
8. the hydrolysis furnace of production fumed silica according to claim 7, which is characterized in that the first gas analysis
Instrument, the second gas analyzer are all made of Zirconium oxide analyzer.
9. the hydrolysis furnace of production fumed silica according to claim 5, which is characterized in that the benefit hydrogen component includes
Hydrogen make pipeline (6), the 4th regulating valve (63), the 4th flowmeter (62),
The hydrogen make pipeline is connect with the middle part of the furnace tube (12), for being passed through hydrogen make-up into furnace tube；
4th regulating valve is set on the hydrogen make pipeline (6), and is connect with the DCS control system (14), is used for
According to the inlet amount information of the hydrogen make-up received, and/or, the letter of the increase/reduction hydrogen make-up inlet amount
Number, itself aperture is adjusted, to control the inlet amount of hydrogen make-up；
4th flowmeter is set on the hydrogen make pipeline (6), for measuring the supplement being passed into the furnace tube
The amount of hydrogen.
10. a kind of system for producing fumed silica, including deacidification furnace, exhaust gas processing device, which is characterized in that further include power
Benefit requires the hydrolysis furnace of the described in any item production fumed silicas of 1-9, and the outlet of the hydrolysis furnace and the deacidification furnace connect
It connects.
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Application publication date: 20191025 |