CN102001670B - Method for producing silicon dioxide by using gas phase process - Google Patents
Method for producing silicon dioxide by using gas phase process Download PDFInfo
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Abstract
The invention relates to a method for producing silicon dioxide by using a gas phase process, which radically solves the problem of high cost of the traditional method for producing the silicon dioxide. The method comprises the steps of: enabling a silicon tetrachloride raw material as a by-product obtained during the production of trichlorosilane, hydrogen and air to enter a combustion reactor respectively by adopting an indirect path and a direct path for reacting to generate silicon dioxide primary particles, wherein the total mol ratio of the silicon tetrachloride raw material to the hydrogen to the air is 1:2.05-7:5.1-198; aggregating the silicon dioxide primary particles through an aggregating device into aggregative state particles, carrying out two stages of cyclone separation of two cyclone separators and spraying and deacidifying through a two-stage air injection deacidifying furnace and entering a bin after deacidifying, and packaging by using vacuum compression; and pre-decontaminating the silicon tetrachloride raw material by using a decontaminating gasifier, wherein the decontaminating gasifier comprises three functional sections of a pre-deslagging section, a gasification section and a high boiling point matter separating section. The invention lowers the production cost on the basis of ensuring the high quality of the silicon dioxide.
Description
Technical field
The present invention relates to the silicon-dioxide correlative technology field of fine inorganic chemicals, specifically a kind of production method of fumed silica.
Background technology
The important source material that vapor phase process is produced in the silicon-dioxide is to be unable to do without the silicon tetrachloride raw material, owing to require higher to the silicon tetrachloride material purity, generally just meeting production requirement more than 99.5%, so manufacturing condition is quite harsh, thereby causes the cost of aerosil high.For reducing the production cost of aerosil, the silicon tetrachloride of by-product was as main raw material when some manufacturers then selected trichlorosilane, because the purity of the silicon tetrachloride of by-product is usually more than 80% when producing trichlorosilane, wherein contain the mechanical impuritys such as outstanding absurd creature and throw out, if adopt common rectificating method as further being purified to more than 99.5%, can the Yin Tanei fouling and high and lowly boil the thing complicated components and produce many insoluble problems.
Can therefore, can utilize the silicon tetrachloride of by-product when producing trichlorosilane, then remove simultaneously and contain low-boiling-point substance, high boiling material, mechanical impurity, be the key point that need to deal with problems.Only so, could use the silicon tetrachloride of by-product when producing trichlorosilane to do raw material, produce high-quality aerosil.So the method how high-quality aerosil is produced in low-cost realization is the direction place that the present invention studies.
Summary of the invention
The purpose of this invention is to provide a kind of production method that can effectively remove the fumed silica of impurities in the silicon tetrachloride raw material and low, high boiling material.Fundamentally solve the existing higher problem of silicon-dioxide production method cost, the silicon-dioxide that adopts the inventive method to make can be used for the purposes identical with commercially available silicon-dioxide, and is guaranteeing to have reduced production cost on the high-quality basis of silicon-dioxide.
Technical scheme of the present invention is: it includes: the silicon tetrachloride raw material of by-product and hydrogen in the time of will producing trichlorosilane first, air adopt respectively indirect and direct two lines to enter in the combustion reactor take the input amount of total mol ratio as 1: 2.05～7: 5.1～198, indirectly enter and refer to: silicon tetrachloride raw material and part air are introduced into impurity-cleaning gasifier after removal of impurities, enter again combustion reactor, its Air inlet accounts for 1/5～1/15 of total air, and the service temperature of impurity-cleaning gasifier is in the 45-90 scope; And hydrogen and residual air capacity directly enter in the combustion reactor;
Silicon tetrachloride and hydrogen, air put in the combustion reactor continuously with above-mentioned mol ratio react, temperature of reaction is 1000～1200 ℃, reaction generates the silicon-dioxide primary particle, and the combustion reactor temperature out is that 200～300 ℃, top hole pressure are in 99.5-101 kPa of scope; This resultant of reaction becomes the state of aggregation particle through aggregator aggregates, two stage cyclone through two cyclonic separators separates and two-stage air-injection deacidification furnace E injection depickling, depickling temperature in the deacidification furnace is 500-600 ℃, arrives feed bin after the depickling, is finished product after packing with vacuum compression; System pressure is controlled in the 85-101 kPa of scope, and the collector temperature in is 100-300 ℃;
Described impurity-cleaning gasifier structure is: comprise pre-slagging-off section, gasification section, high boiling material segregation section three functions section, described three functions section connects successively, described pre-slagging-off section can be formed and each top, described deslagging unit is interconnected by a plurality of deslagging units in series, the top, described deslagging unit of described pre-slagging-off section front end arranges the liquid starting material opening for feed, the top, described deslagging unit of rear end arranges the low-boiling-point substance relief outlet, and the slag charge outlet of each described deslagging unit bottom all connects slag off apparatus; Described gasification section arranges gasification section Flow of Goods and Materials chamber, the material inlet in described gasification section Flow of Goods and Materials chamber is described pre-slagging-off section material outlet, the material outlet in described gasification section Flow of Goods and Materials chamber is the material inlet of described high boiling material segregation section, and described gasification section Flow of Goods and Materials arranges interceptor in the chamber; Described high boiling material segregation section comprises gas-liquid separator, exports the high boiling material escaper that is connected with the high boiling material of described gas-liquid separator bottom, and described gas-liquid separator top is provided with gaseous phase materials and exports; Described pre-slagging-off section, gasification section, the high boiling material segregation section three functions section cavity outside are respectively equipped with heating jacket.
Air spray depickling after the cyclonic separation of the second stage directly enters in the deacidification furnace or turns back to the entrance of first step cyclonic separation.
Air enters described combustion reactor after the air preheater preheating, preheating temperature is 100-200 ℃.
The described slag off apparatus top of described pre-slagging-off section arranges liquid starting material material-feeding port and balance port, described slag off apparatus below arranges slag-drip opening, and the slag charge exit of described liquid starting material material-feeding port, balance port, slag-drip opening and described deslagging unit bottom arranges respectively valve.
The overflow weir that some regulator solution streams distribute is set on the liquid-flow face of the gasification section of the bottom, gasification section Flow of Goods and Materials chamber of described gasification section, and the liquid-flow face of the liquid-flow face of described gasification section and pre-slagging-off section is along liquid flow direction horizontal by the angle of declination state.
The described high boiling material escaper top of described high boiling material segregation section arranges balance port, described high boiling material escaper below arranges the high boiling material discharge outlet, and the high boiling material exit of described balance port, high boiling material discharge outlet and described gas-liquid separator bottom arranges respectively valve.
The described liquid starting material opening for feed place of described pre-slagging-off section front end is provided with the liquid spraying divider.
A described pre-slagging-off section front end arranges carrier gas inlet, described carrier gas inlet place be provided with prevent liquid material drench into baffle plate.
In the described deslagging unit cavity of described pre-slagging-off section filler and the baffle plate that stops the dregs back-mixing is set, is provided with the filler that is beneficial to gas-liquid separation in the gas-liquid separator cavity of described high boiling material segregation section.
Described slag off apparatus and described high boiling material escaper arrange respectively the cleaning operation hand hole.
Advantage of the present invention and positive technique effect are: the by-product silicon tetrachloride when the present invention has adopted the production trichlorosilane in its production method is as raw material, thereby greatly reduce the raw materials cost of producing high quality silicon-dioxide, simultaneously, in order to guarantee the high quality of by-product silicon tetrachloride, the present invention has adopted specially designed impurity-cleaning gasifier to its in advance removal of impurities, guarantees the purity when it participates in reaction; In addition, because silicon tetrachloride has strong toxicity, severe corrosive, excessive as the byproduct of trichlorosilane, be difficult to process, so also highly beneficial for producing this Chemicals of trichlorosilane.So adopting the by-product silicon tetrachloride when producing trichlorosilane when producing aerosil is the technical scheme of achieving many things at one stroke as raw material, for the production of aerosil and two kinds of Chemicals of trichlorosilane has all brought huge benefit, it has great economy and environment protection significance.
Description of drawings
Fig. 1 is technique simplified schematic diagram of the present invention;
Fig. 2 is gasifier of the present invention (finishing the interior partial function of two dot chain line frame among Fig. 1) structural representation sketch.
Sequence number explanation among the figure:
Fig. 1: A vaporizer, B oxyhydrogen combustion reactor, C collector, D cyclonic separator group, E deacidification furnace, F finished product bin, G wrapping machine; A1 air, a2 raw material silicon tetrachloride, a3 mechanical impurity, a4 high boiling material, a5 silicon tetrachloride vapor, a6 low-boiling-point substance, b1 chlorine, b2 air, d1 tail gas, e1 air, e2 slag charge, e3 tail gas, f1 tail gas, the packed one-tenth mouth of g1;
Fig. 2: I is the section of slagging-off, II gasification section, III high boiling material segregation section in advance;
1 carrier gas inlet, 2 liquid starting material opening for feeds, 3 pre-slagging-off section liquid-flow faces, 4 filler, 5 low-boiling-point substance relief outlets, 6 heating jackets, 7 gasification section Flow of Goods and Materials chambeies, 8 interceptors, 9 useful gaseous phase materials outlets, 10 gas-liquid separators, the outlet of 11 high boiling material, 12 balance port, 13 high boiling material escapers, 14 high boiling material discharge outlets, 15 gasification section material outlets (material inlet of high boiling material segregation section), 16 overflow weirs, the liquid-flow face of 17 gasification section, 18 pre-slagging-off section material outlets (gasification section material inlet), 19 baffle plates, 20 balance port, 21 slag off apparatuss, 22 slag-drip openings, 23 liquid starting material material-feeding ports, 24 deslagging unit slag charge outlets (slag off apparatus entrance), 25 heating jackets, 26 deslagging unit, 27 liquid spraying dividers, 28 carrier gas inlet baffle plates, 29 heating jackets.
Embodiment
According to Fig. 1-2 technical scheme of the present invention is described in detail.
As shown in Figure 1, the present invention, the mol ratio that enters the silicon tetrachloride a2 of combustion reactor B and hydrogen b1, air is 1: 2.05～7: 5.1～198.Silicon tetrachloride a2 and hydrogen b1, air adopt respectively indirect and direct two lines to enter among the combustion reactor B, being specially air is added by air a1 and air b2 two lines respectively, wherein added the air of system by air a1 circuit, account for 1/5～1/15 of total air.And hydrogen b1 and residual air capacity directly enter among the combustion reactor B.
As shown in Figure 1, raw material silicon tetrachloride a2 and air a1 enter impurity-cleaning gasifier A after metering, and the silicon tetrachloride after the gasification enters 1000～1200 ℃ of combustion reactor B that oxyhydrogen flame is arranged, and carries out mechanism reaction schematically as follows:
SiCl
4+2H
2+O
2＝SiO
2+4HCl
Silicon tetrachloride sprays in above-mentioned indirect and direct mode with air, hydrogen and mixes, silicon tetrachloride and hydrogen, air put among the combustion reactor B continuously with above-mentioned mol ratio react, reaction generates the silicon-dioxide primary particle, this particle generates chain-like structure condense collision in collector C after, further is gathered into to have cancellated state of aggregation particle again.Through the white carbon black of agglomeration separation twin-stage spray can be continuous in the process unit of depickling in deacidification furnace E, finish deacidification.This twin-stage sprays to spray by one-level isolate is sprayed in the deacidification furnace E, and simultaneously two-stage injection is to guarantee further replenishing of one-level injection, realize the circulation recovery, thereby the yield that has guaranteed cyclonic separator D reaches more than 99%.Finished product of the present invention adopts the vacuum compression packing technique, and white carbon black is entered among the Vacuum Packaging Machine G by finished pot, is provided with scraper in the outlet of compressor, the white carbon black finished product is scraped enter among the wrapping machine G, contracts out finished product by wrapping machine G again.
Wherein, combustion reaction temperature is controlled at 1000～1200 ℃, combustion reactor B temperature out be 200～300 ℃, top hole pressure in 99.5-101 kPa of scope, this resultant of reaction is gathered into the state of aggregation particle through collector C, collector C temperature in is 100-300 ℃.Two stage cyclone through two cyclonic separator D separates and two-stage air-injection deacidification furnace E injection depickling again, depickling temperature in the deacidification furnace E is 500-600 ℃, namely about 550 ℃, arrive feed bin F after the depickling, be packaged into the packed commodity of 10kg with wrapping machine G and be finished product, system pressure is controlled in the 85-101 kPa of scope.
Referring to Fig. 2, impurity-cleaning gasifier A is the distinctive gasifier of the present invention, the low-boiling-point substance that is widely used in containing in the system and the boiling point of high boiling material and the rear useful component boiling-point difference liquid material system larger and that contain mechanical impurity of utilizing of needs gasification use as the gasifier that has slagging-off, purification, gasification function concurrently.The service temperature of impurity-cleaning gasifier A of the present invention is in the 45-90 scope, can be at the mechanical impurity and the low-boiling-point substance that separate below 45-56 ℃ in the raw material silicon tetrachloride, separating high boiling material more than 57-90 ℃, thereby make raw material silicon tetrachloride purity reach requirement, guarantee to produce stable carrying out, guarantee that product purity and application performance meet the requirements.Its structure mainly is comprised of pre-slagging-off section I, gasification section II, high boiling material segregation section III three functions section, this three functions section connects successively, and pre-slagging-off section I, gasification section II, the high boiling material segregation section III three functions section cavity outside are respectively equipped with heating jacket 25,6,29.
Pre-slagging-off section I can be in series and each 26 tops, deslagging unit are interconnected by a plurality of deslagginves unit 26.The position that is interconnected, each deslagging unit 26 is provided with the liquid-flow face 3 of pre-slagging-off section.26 tops, front and back ends deslagging unit of pre-slagging-off section arrange respectively liquid starting material opening for feed 2 and low-boiling-point substance relief outlet 5, according to liquid material characteristic and processing requirement, can carrier gas inlet 1 be set at pre-slagging-off section front end.The shape of deslagging unit is not particularly limited, and can be cylindric or quadrangular shape etc., can set as required, and when its cavity horizontal section when being cylindric, liquid material can adopt tangential direction to enter.All arrange in each deslagging unit 26 cavity and reduce back-mixing filler 4 effect, that be conducive to dreg settling and anti-back-mixing umbrella or carinate baffle plate 19.
Gasification section II arranges gasification section Flow of Goods and Materials chamber 7, and the material inlet 18 in gasification section Flow of Goods and Materials chamber is pre-slagging-off section material outlet, and the material outlet 15 in gasification section Flow of Goods and Materials chamber is the material inlet of high boiling material segregation section.
High boiling material segregation section III is mainly by gas-liquid separator 10, form with the high boiling material of gas-liquid separator 10 bottoms outlet 11 high boiling material escapers 13 that are connected etc.At high boiling material segregation section III, high boiling material is accumulated in gas-liquid separator 10 bottoms and the high boiling material escaper 13 after useful component gasification.Gas-liquid separator 10 tops are provided with gaseous phase materials outlet 9, and the useful component steam after the purification and carrier gas are by this mouthful output.Be provided with the filler that is beneficial to gas-liquid separation in gas-liquid separator 10 cavitys, add filler and can eliminate the problem that liquid is walked by gas entrainment.High boiling material escaper 13 tops arrange balance port 12, and high boiling material escaper 13 belows arrange high boiling material discharge outlet 14, and the high boiling material of balance port 12, high boiling material discharge outlet 14 and gas-liquid separator bottom exports 11 places valve is set respectively.The slag off apparatus 21 of pre-slagging-off section I and the high boiling material escaper 13 of high boiling material segregation section III arrange respectively the cleaning operation hand hole.
As shown in Figure 2, the silicon tetrachloride a2 liquid state of by-product enters impurity-cleaning gasifier A of the present invention when producing trichlorosilane low-boiling-point substance and the mechanical impurity section of removing, air a1 also adds impurity-cleaning gasifier A as carrier gas.Silicon tetrachloride and air can first preheatings, and low-boiling-point substance and mechanical impurity remove the intersegmental part temperature and be controlled at below 56 ℃; The material that has removed low-boiling-point substance a6 and mechanical impurity a3 enters into the gasification section of impurity-cleaning gasifier A, makes silicon tetrachloride vaporization and separates high boiling material a4; The vaporization section internal temperature is controlled at more than 57 ℃.Silicon tetrachloride a5 after the purification and hydrogen b1, air b2 are together sent to and are carried out reaction shown in Figure 1 among the combustion reactor B.Concrete removal of impurities process is as follows:
At pre-slagging-off section I, mechanical impurity and low-boiling-point substance are removed.The slag charge outlet 24 of each 26 bottom, deslagging unit all connects slag off apparatus 21, and slag off apparatus 21 tops arrange liquid starting material material-feeding port 23 and balance port 20, and slag off apparatus 21 belows arrange slag-drip opening 22.The slag charge of liquid starting material material-feeding port 23, balance port 20, slag-drip opening 22 and deslagging unit bottom exports 24 places valve is set respectively.Raw material liq adds from liquid starting material opening for feed 2, the liquid starting material opening for feed can be provided with the liquid spraying divider 27 of sprinkle nozzle or other form for 2 times, carrier gas (can be one of raw material) enters from carrier gas inlet 1, and carrier gas inlet 1 place also can arrange narrow slit type divider or baffle plate 28.Gas is with after liquid contacts, and mechanical impurity continues sedimentation, enters slag off apparatus 21 by deslagging unit slag charge outlet (slag off apparatus entrance) 24.Discharging is closed first deslagging unit slag charge outlet (slag off apparatus entrance) 24 place's valves during slag charge, opens balance port 20 place's valves, opens slag-drip opening 22 place's valves slag charge of draining.After the slag charge emptying, close slag-drip opening 22 place's valves, open liquid starting material material-feeding port 23 place's valves and replenish full slag off apparatus 21, then closing liquid raw material material-feeding port 23 place's valves and balance port 20 place's valves are opened deslagging unit slag charge outlet (slag off apparatus entrance) 24 place's valves at last;
At gasification section II, useful component is vaporized with high boiling material and realizes separating.The material of removing behind mechanical impurity and the low-boiling-point substance enters from the material inlet 18 in gasification section Flow of Goods and Materials chamber, and the flow through liquid-flow face 17 of gasification section of liquid, useful component were vaporized arrive the material outlet 15 in gasification section Flow of Goods and Materials chamber at material before.The flow distribution of liquid phase material on liquid-flow face 17 of becoming reconciled for the gaseous phase materials admixture that obtains, the gasification section Flow of Goods and Materials chamber 7 interior interceptors 8 that arrange arrange the overflow weir 16 that some regulator solution streams distribute on the mobile face 17 of gasification section Flow of Goods and Materials chamber bottom liquid.Interceptor 8 shapes are set as required.The liquid-flow face 3 of pre-slagging-off section and the liquid-flow face 17 of gasification section are along liquid flow direction horizontal by the angle of declination state, and the inclination angle scope is greatly about 0-25 °, so that liquid-flow;
When high boiling material segregation section III discharging high boiling material, close the valve that high boiling material exports 11 places, open balance port 12 place's valves, open again the valve at high boiling material discharge outlet 14 places, but the emptying high boiling material.Then, close high boiling material discharge outlet 14 place's valves, the valve of closing balance port 12 places is opened the valve that high boiling material exports 11 places at last, continues to accumulate high boiling material.
Embodiment 1
In hydrogen: silicon tetrachloride: air=1: 1.6 * 10-3: 1.5 (mol ratio) ratio, three kinds of materials of aforementioned base materials silicon tetrachloride, hydrogen, air that will contain silicon tetrachloride 90.5% are sent into combustion reactor 2 with aforementioned manner.Through obtaining product analysis (according to Q/SHG19-2008) result after the technological process shown in Figure 1 be:
Specific surface area: 142m
2/ g
PH value: 3.8
Apparent density: 53g/l.
Claims (10)
1. the production method of a fumed silica, it includes: the silicon tetrachloride raw material of by-product and hydrogen in the time of will producing trichlorosilane first, air adopt respectively indirect and direct two lines to enter in the combustion reactor take the input amount of total mol ratio as 1: 2.05～7: 5.1～198, indirectly enter and refer to: silicon tetrachloride raw material and part air are introduced into impurity-cleaning gasifier after removal of impurities, enter again combustion reactor, wherein above-mentioned part air inlet accounts for 1/5～1/15 of total air, and the service temperature of impurity-cleaning gasifier is in 45-90 ℃ of scope; And hydrogen and residual air capacity directly enter in the combustion reactor;
Silicon tetrachloride and hydrogen, air put in the combustion reactor continuously with above-mentioned mol ratio react, temperature of reaction is 1000～1200 ℃, reaction generates the silicon-dioxide primary particle, and the combustion reactor temperature out is that 200～300 ℃, top hole pressure are in 99.5-101 kPa of scope; This resultant of reaction becomes the state of aggregation particle through aggregator aggregates, two stage cyclone through two cyclonic separators separates and two-stage air-injection deacidification furnace E injection depickling, depickling temperature in the deacidification furnace is 500-600 ℃, arrives feed bin after the depickling, is finished product after packing with vacuum compression; System pressure is controlled in the 85-101 kPa of scope, and the collector temperature in is 100-300 ℃;
Described impurity-cleaning gasifier structure is: comprise pre-slagging-off section, gasification section, high boiling material segregation section three functions section, described three functions section connects successively, described pre-slagging-off section is formed by a plurality of deslagging units in series and each top, described deslagging unit is interconnected, the top, described deslagging unit of described pre-slagging-off section front end arranges the liquid starting material opening for feed, the top, described deslagging unit of rear end arranges the low-boiling-point substance relief outlet, and the slag charge outlet of each described deslagging unit bottom all connects slag off apparatus; Described gasification section arranges gasification section Flow of Goods and Materials chamber, the material inlet in described gasification section Flow of Goods and Materials chamber is described pre-slagging-off section material outlet, the material outlet in described gasification section Flow of Goods and Materials chamber is the material inlet of described high boiling material segregation section, and described gasification section Flow of Goods and Materials arranges interceptor in the chamber; Described high boiling material segregation section comprises gas-liquid separator, exports the high boiling material escaper that is connected with the high boiling material of described gas-liquid separator bottom, and described gas-liquid separator top is provided with gaseous phase materials and exports; Described pre-slagging-off section, gasification section, the high boiling material segregation section three functions section cavity outside are respectively equipped with heating jacket.
2. the production method of a kind of fumed silica according to claim 1, it is characterized in that: the air spray depickling after the cyclonic separation of the second stage directly enters in the deacidification furnace or turns back to the entrance of first step cyclonic separation.
3. the production method of a kind of fumed silica according to claim 1, it is characterized in that: air enters described combustion reactor after the air preheater preheating, and preheating temperature is 100-200 ℃.
4. the production method of a kind of fumed silica according to claim 1, it is characterized in that: the described slag off apparatus top of described pre-slagging-off section arranges liquid starting material material-feeding port and balance port, described slag off apparatus below arranges slag-drip opening, and the slag charge exit of described liquid starting material material-feeding port, balance port, slag-drip opening and described deslagging unit bottom arranges respectively valve.
5. the production method of a kind of fumed silica according to claim 1, it is characterized in that: the overflow weir that some regulator solution streams distribute is set on the liquid-flow face of the gasification section of the bottom, gasification section Flow of Goods and Materials chamber of described gasification section, and the liquid-flow face of the liquid-flow face of described gasification section and pre-slagging-off section is along liquid flow direction horizontal by the angle of declination state.
6. the production method of a kind of fumed silica according to claim 1, it is characterized in that: the described high boiling material escaper top of described high boiling material segregation section arranges balance port, described high boiling material escaper below arranges the high boiling material discharge outlet, and the high boiling material exit of described balance port, high boiling material discharge outlet and described gas-liquid separator bottom arranges respectively valve.
7. it is characterized in that according to claim 1 or the production method of 4 described a kind of fumed silicas: the described liquid starting material opening for feed place of described pre-slagging-off section front end is provided with the liquid spraying divider.
8. according to claim 1 or the production method of 4 described a kind of fumed silicas, it is characterized in that: a described pre-slagging-off section front end arranges carrier gas inlet, described carrier gas inlet place be provided with prevent liquid material drench into baffle plate.
9. according to claim 1 or the production method of 4 or 6 described a kind of fumed silicas, it is characterized in that: in the described deslagging unit cavity of described pre-slagging-off section filler and the baffle plate that stops the dregs back-mixing is set, is provided with the filler that is beneficial to gas-liquid separation in the gas-liquid separator cavity of described high boiling material segregation section.
10. according to claim 1 or 4 or 6 or the production method of described a kind of fumed silica, it is characterized in that: described slag off apparatus and described high boiling material escaper arrange respectively the cleaning operation hand hole.
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| CN102267701B (en) * | 2011-06-30 | 2013-01-30 | 中煤平朔煤业有限责任公司 | Device for continuously producing white carbon black |
| CN107973546A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | One kind well cementation oil-well cement suspending agent and preparation method thereof and cement paste for well cementation |
| CN111484022B (en) * | 2019-12-23 | 2022-12-06 | 浙江精功新材料技术有限公司 | White carbon black combustion furnace structure |
| CN113493674A (en) * | 2020-03-19 | 2021-10-12 | 佛山市顺德区天采有机硅有限公司 | Strong structural adhesive and preparation method thereof |
| CN112569735A (en) * | 2020-11-27 | 2021-03-30 | 株洲宏大高分子材料有限公司 | Method and device for removing sulfuric acid smoke in tail gas pipeline of flue gas acid making system |
| CN112723364B (en) * | 2020-12-31 | 2022-12-13 | 徐小岗 | Method for producing high-activity high-purity fumed silica |
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| CN1208016A (en) * | 1998-08-27 | 1999-02-17 | 沈阳化工股份有限公司 | Gas phase process preparing white carbon |
| CN1850599A (en) * | 2006-04-29 | 2006-10-25 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN101734668A (en) * | 2009-12-28 | 2010-06-16 | 周庆华 | Method for preparing white carbon black by gas phase method and used equipment thereof |
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| CN1208016A (en) * | 1998-08-27 | 1999-02-17 | 沈阳化工股份有限公司 | Gas phase process preparing white carbon |
| CN1850599A (en) * | 2006-04-29 | 2006-10-25 | 广州吉必时科技实业有限公司 | Comprehensive utilization method of by-product for poycrystalline silicon production process |
| CN101734668A (en) * | 2009-12-28 | 2010-06-16 | 周庆华 | Method for preparing white carbon black by gas phase method and used equipment thereof |
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