CN101734668A - Method for preparing white carbon black by gas phase method and used equipment thereof - Google Patents
Method for preparing white carbon black by gas phase method and used equipment thereof Download PDFInfo
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- CN101734668A CN101734668A CN200910265416A CN200910265416A CN101734668A CN 101734668 A CN101734668 A CN 101734668A CN 200910265416 A CN200910265416 A CN 200910265416A CN 200910265416 A CN200910265416 A CN 200910265416A CN 101734668 A CN101734668 A CN 101734668A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides equipment for preparing white carbon black by a gas phase method and a method for preparing the white carbon black by using the equipment. The equipment successively comprises a raw material preheater, a raw material mixer, an injecting device and a high temperature hydrolysis furnace, and is characterized in that the part between the injecting device and the high temperature hydrolysis furnace are connected and sealed by a seal connecting piece, and the injecting device is arranged between the raw material mixer and the high temperature hydrolysis furnace.In the high temperature hydrolysis furnace of the invention, the seal combustion technology, the water cooling jacket type cooling technology, the unique deacidification technology and the advanced filtering technology are utilized, so that the obtained white carbon black has small fluctuation on the special surface area, the production efficiency is improved and the energy is saved greatly.
Description
Technical field
The invention belongs to inorganic fine chemical technology field, particularly, relate to a kind of preparation method of thermal silica and the equipment of use thereof.
Background technology
Thermal silica is developed in nineteen forty-one by German Degussa Corporation the earliest, at present only virtuous, beautiful in the world, day, black, suitability for industrialized production technology that medium a few countries has been grasped thermal silica.Currently used thermal silica production technique all is earlier the silicon alkyl halide of vaporization and hydrogen, air mixed mostly, then under the uncovered condition in pyrohydrolysis stove (also can be described as Reaktionsofen or roasting kiln etc.) reaction generate gas-phase silica and hydrogenchloride, separate again at last and make finished product.This method adopts uncovered mode combustion hydrolytic, and the extraneous air that replenishes contains impurity and can't measure, and causes the specific surface area fluctuation of finished product bigger, influences quality product.In addition, aspect the cooling of pyrohydrolysis stove, mostly adopt powerful roots blower in the prior art, energy consumption is bigger, and the heat energy after the heat exchange is difficult to comprehensive utilization, and amount of cooling water is little, influences the throughput of single covering device.
The subject matter that white carbon black production technology of the prior art exists is: (1) raw material in the pyrohydrolysis stove under the uncovered condition combustion hydrolytic cause the specific surface area fluctuation of white carbon black bigger, the quality instability; (2) heat of reaction in the pyrohydrolysis stove can not in time be taken away, and influences single covering device throughput and heat energy and does not make full use of; (3) technology of gas solid separation is not mature enough, contains a large amount of white carbon blacks in the tail gas, causes that easily exhaust system stops up, cause drive unstable, can not continuous production, influence quality product and production efficiency; (4) ability of depickling is not enough, and deacidifying process falls behind, and adopts electric-heating technology mostly, and the depickling ability reduces.
Summary of the invention
The purpose of this invention is to provide method and the used device of this method that a kind of specific surface area fluctuation that can make the gained white carbon black reduces with respect to prior art.
Further, the present invention also aims to provide a kind of can make the heat in the high temperature combustion furnace in time take away, and can be utilized effectively, thereby enhance productivity, production security, and the white carbon black production method of save energy and the equipment of use thereof greatly.
Further, the present invention ground purpose also is to provide a kind of white carbon black and hydrogenchloride white carbon black production method effectively discretely.
To achieve these goals, the invention provides a kind of equipment that is used to prepare thermal silica, it comprises feed preheater, material mixer, jet apparatus and pyrohydrolysis stove successively, it is characterized in that, be tightly connected by a seal connector between described jet apparatus and the described pyrohydrolysis stove, and described jet apparatus is between described material mixer and described pyrohydrolysis stove.
Preferably, the pyrohydrolysis stove in the equipment of the present invention is connected with an electronic ignition device, by this electronic ignition device igniting causing material combusting reaction.
Preferably, the seal connector in the equipment of the present invention is a flange.
Preferably, the pyrohydrolysis stove in the equipment of the present invention comprises shaft and is positioned at the outer chuck of shaft, and is connected with water coolant in the described chuck, so that heat of reaction not only can in time remove, and helps the heat energy recycle of subsequent step.Preferred in addition, described shaft is made by the titanium material, and described chuck is made by carbon steel, reduces investment.
Preferably, the downstream of the pyrohydrolysis stove of equipment of the present invention further is connected with monobromination lithium unit, described lithiumbromide unit has pyrohydrolysis stove hot water (about 98～100 ℃) inlet, inferior hot water (about 75～85 ℃) outlet, water coolant (about 25-30 ℃) inlet, water coolant (about 45～55 ℃) outlet, refrigerated water (about 2-5 ℃) outlet, freezing backwater (about 8～10 ℃) inlet, enter into the lithiumbromide unit by the pyrohydrolysis stove hot water that comes out in the pyrohydrolysis stove chuck, and the heat energy that relies on this pyrohydrolysis stove hot water to produce drives the running of lithiumbromide unit, so that the freezing backwater (about 8～10 ℃) that the lithiumbromide unit will enter wherein further is cooled to refrigerated water (about 2-5 ℃), in squeezing into the heat exchanger of tail gas, recycle pump is used for the tail gas cooling, a part becomes time hot water after driving lithiumbromide, come back in the chuck of pyrohydrolysis stove, cooling down high-temperature hydrolysis stove, the water coolant of lithiumbromide unit returns the lithiumbromide unit and recycles through cooling off to water cooling tower after the heat exchange.The present invention has not only improved production efficiency with this structure that the pyrohydrolysis stove is connected with the lithiumbromide unit, has guaranteed production security, and has fully realized effective utilization of the energy,
The pyrohydrolysis stove of equipment of the present invention, its downstream further are connected with gas-solid separator, cloth bag separator and rotary kiln deacidifying device, and the gas-phase silica that is used for generating separates with hydrogenchloride.The present invention makes the hydrogenchloride that is coated on the white carbon black effectively separate by this stage trapping system, thereby has guaranteed the quality of the gas-phase silica that generated.
The present invention also provides a kind of preparation method of thermal silica, has wherein used aforementioned device.
The present invention also provides a kind of preparation method of thermal silica, comprises the steps:
(1) according to the predetermined proportion charging;
(2) raw material preheating: respectively with raw silicon halogen compound, hydrogen and preheating of air;
(3) raw material mixes: the raw material after the preheating is mixed;
(4) spray: with mixed raw material through the nozzle ejection of injector in the pyrohydrolysis stove, be tightly connected by a seal connector between wherein said injector and the described pyrohydrolysis stove, thereby guaranteed that the material rate that enters in the described pyrohydrolysis stove is consistent with predetermined proportion;
(5) high-temperature hydrolysis: the raw material that enters in the pyrohydrolysis stove is lighted a fire through electronic ignition device, and reaction generates the mixture that contains gas-phase silica and hydrogen chloride gas;
(6) product separates, and collects.
Preferably, between the step (2) of aforesaid method and (3), also comprise a step that silicon halogen compounds is boiled again.
Preferably, in above-mentioned preparation method, the downstream of described pyrohydrolysis stove further is connected with monobromination lithium unit, realizes the recycling of the heat energy that the pyrohydrolysis stove produces by this lithiumbromide unit.
Preferably, in above-mentioned preparation method, wherein said product separating step comprises that the mixture that high temperature combustion furnace is come out at first carries out gas solid separation by a common gas-solid separator, further separate through a cloth bag separator then, thoroughly separate by single-revolution kiln deacidifying device more at last.
Preferably, among the above-mentioned again preparation method, described silicon halogenide is selected from one or more in monomethyl trichlorosilane, dimethyldichlorosilane(DMCS), tri-methyl-chlorosilane, monomethyl dichloro silicon fluoride, propyltrichlorosilan, two fourth dimethyl dichlorosilane (DMCS)s, basic trichlorosilane, trichlorosilane, the silicon tetrachloride.
Single covering device of the present invention has the throughput of 2500T/a, adopts technology of the present invention to improve quality product, output, has reduced investment, has accomplished effective recycle of heat energy, has improved production efficiency.Method of the present invention is that the halogenide of thermal pretreatment, air and hydrogen are carried out the combustion hydrolytic reaction in the airtight pyrohydrolysis stove of input of continous-stable in proportion, entire reaction is carried out in confined conditions, need not to replenish air in the reaction process, pass through electronic ignition device, light reaction hydrogen, material is carried out under the influence that is not subjected to extraneous factor in proportion continuously and stably, make that the surface-area fluctuation of gained white carbon black is less.Simultaneously, reaction a large amount of heats of emitting are taken away by the water in the chuck, and heated water enters monobromination lithium unit and carried out the conversion of energy in chuck, thereby have realized safe and efficient production on the one hand, have also realized effective utilization of the energy on the one hand.
Description of drawings
The preparation facilities synoptic diagram that is adopted among the preparation method of Fig. 1 embodiment 1.
Description of reference numerals:
1: air preheater 2: hydrogen preheater 3: the silane preheater
4: mix Venturi 5: jet apparatus 6: silane reboiler
7: airtight junctor 8: pulse igniter 9: pyrohydrolysis stove
10: cooling transverse tube 11: gas-solid separator 12: sack cleaner
13: hydrochloric acid absorption tower 14: water cooler 15: the lithiumbromide unit
16: depickling stove 17: feed bin 18: wrapping machine
T1: pyrohydrolysis stove hot water T2: inferior hot water T3: cooling water inlet
T4: cooling water outlet T5: chilled water outlet T6: freezing backwater inlet
Embodiment
Embodiment 1
In 2: (0.8-1.1): (20-25): ratio (2-3) is accurately measured silicon tetrachloride, air and hydrogen respectively, silicon tetrachloride is vaporized through silane reboiler 6 after 3 preheatings of silane preheater again, mix in mixing Venturi 4 with air then from air preheater 1, mixed raw material mixes in jet apparatus 5 with hydrogen from hydrogen preheater 2 after carry out high-temperature hydrolysis by the nozzle ejection of this jet apparatus 5 in pyrohydrolysis stove 9, generates a large amount of gas-phase silica gas-solid mixtures and discharges a large amount of heats.Wherein be connected by flange seal between jet apparatus 5 and the pyrohydrolysis stove 9, and do not replenish air spraying mix stages and pyrohydrolysis stage.The gas-solid mixture of discharging from pyrohydrolysis stove 9 is at first through 10 coolings of overcooling transverse tube, be separated into white carbon black part and hydrogenchloride part via gas-solid separator 11 and sack cleaner 12 then, wherein the white carbon black part is further gone into feed bin 17 except that hydrogenchloride is laggard via depickling stove 16, at last by wrapping machine 18 packings, after hydrogenchloride partly passes through hydrochloric acid absorption tower 13, discharge hydrochloric acid, emit a large amount of heat during hydrochloric acid, further cool off by water cooler 14.As shown in fig. 1, the reactor shown in the present embodiment can also be connected with monobromination lithium unit 15, to realize effective utilization of the energy.
After testing, its particle diameter of the white carbon black of gained remains between the 20nm-50nm good product dispersibility in the present embodiment.
Comparative example 1
Other condition is identical with embodiment 1, difference only be mixed raw material through the nozzle of injector under open state, spurt in the pyrohydrolysis stove and react.
After testing, the particle diameter of products obtained therefrom is in the 50nm-200nm scope in this example, and product is dispersed relatively poor.
Claims (10)
1. equipment that is used to prepare thermal silica, it comprises feed preheater, material mixer, jet apparatus and pyrohydrolysis stove successively, it is characterized in that, be tightly connected by a seal connector between described jet apparatus and the described pyrohydrolysis stove, and described jet apparatus is between described material mixer and described pyrohydrolysis stove.
2. the described equipment of claim 1 is characterized in that wherein said pyrohydrolysis stove is connected with an electronic ignition device.
3. the described equipment of claim 1 is characterized in that wherein said pyrohydrolysis stove comprises shaft and is positioned at the outer chuck of shaft, and is connected with water coolant in the described chuck.
4. each described equipment of claim 1～3, the downstream that it is characterized in that wherein said pyrohydrolysis stove further is connected with monobromination lithium unit, described lithiumbromide unit has pyrohydrolysis stove hot water inlet, inferior hot water outlet, the cooling water inlet, cooling water outlet, chilled water inlet and chilled water outlet, enter into the lithiumbromide unit by the pyrohydrolysis stove hot water that comes out in the pyrohydrolysis stove chuck, and the heat energy that relies on this pyrohydrolysis stove hot water to produce drives the running of lithiumbromide unit, so that the freezing backwater (about 8～10 ℃) that the lithiumbromide unit will enter wherein further is cooled to refrigerated water (about 2-5 ℃), in squeezing into the heat exchanger of tail gas, recycle pump is used for the tail gas cooling, a part becomes time hot water after driving lithiumbromide, come back in the chuck of pyrohydrolysis stove, cooling down high-temperature hydrolysis stove, the water coolant of lithiumbromide unit returns the lithiumbromide unit and recycles through cooling off to water cooling tower after the heat exchange.
5. each described equipment of claim 1～4 is characterized in that the downstream of wherein said pyrohydrolysis stove further is connected with gas-solid separator, cloth bag separator and rotary kiln deacidifying device, and the white carbon black that is used for generating separates with hydrogenchloride.
6. the preparation method of a thermal silica is characterized in that using each described equipment of claim 1～5.
7. the preparation method of a thermal silica is characterized in that comprising the steps:
(1) according to the predetermined proportion charging;
(2) raw material preheating: respectively with raw silicon halogen compound, hydrogen and preheating of air;
(3) raw material mixes: the raw material after the preheating is mixed;
(4) spray: with mixed raw material through the nozzle ejection of injector in the pyrohydrolysis stove, be tightly connected by a seal connector between wherein said injector and the described pyrohydrolysis stove, thereby guaranteed that the material rate that enters in the described pyrohydrolysis stove is consistent with predetermined proportion;
(5) high-temperature hydrolysis: the raw material that enters in the pyrohydrolysis stove is lighted a fire through electronic ignition device, and reaction generates the mixture that contains gas-phase silica and hydrogen chloride gas;
(6) product separates, and collects.
8. the described preparation method of claim 7 is characterized in that wherein also comprising a step that silicon halogen compounds is boiled again between step (2) and (3); Or the downstream of wherein said pyrohydrolysis stove further is connected with monobromination lithium unit, realizes the recycling of the heat energy that pyrohydrolysis stove produces by this lithiumbromide unit.
9. each described preparation method of claim 7～8, wherein said product separating step comprises that the mixture that high temperature combustion furnace is come out at first carries out gas solid separation by a common gas-solid separator, further separate through a cloth bag separator then, thoroughly separate by single-revolution kiln deacidifying device more at last.
10. according to each described preparation method of claim 7～9, it is characterized in that wherein said silicon halogenide is selected from one or more in monomethyl trichlorosilane, dimethyldichlorosilane(DMCS), tri-methyl-chlorosilane, monomethyl dichloro silicon fluoride, propyltrichlorosilan, two fourth dimethyl dichlorosilane (DMCS)s, hexyl trichlorosilane, trichlorosilane, the silicon tetrachloride.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910265416A CN101734668A (en) | 2009-12-28 | 2009-12-28 | Method for preparing white carbon black by gas phase method and used equipment thereof |
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| CN200910265416A CN101734668A (en) | 2009-12-28 | 2009-12-28 | Method for preparing white carbon black by gas phase method and used equipment thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001670A (en) * | 2010-10-29 | 2011-04-06 | 沈阳化工股份有限公司 | Method for producing silicon dioxide by using gas phase process |
| CN102476802A (en) * | 2010-11-23 | 2012-05-30 | 北京航天赛德科技发展有限公司 | Preparation method of silica used for leather delustering agent and its device |
| CN102583396A (en) * | 2012-03-08 | 2012-07-18 | 上海竟茨环保科技有限公司 | Deacidification equipment for producing fumed silica |
| CN104628005A (en) * | 2013-11-07 | 2015-05-20 | 浙江开化合成材料有限公司 | Vaporizer, white carbon black production apparatus and white carbon black production method |
| CN106241821A (en) * | 2016-07-21 | 2016-12-21 | 宜昌南玻硅材料有限公司 | The mixing arrangement of a kind of nanoscale fume colloidal silica raw material and method |
| CN107777693A (en) * | 2017-11-14 | 2018-03-09 | 宜昌汇富硅材料有限公司 | The production technology and device of a kind of nano fumed silica |
| CN108190950A (en) * | 2018-02-06 | 2018-06-22 | 新疆晶硕新材料有限公司 | The preparation method and device of zirconium dioxide |
| CN108585038A (en) * | 2018-04-13 | 2018-09-28 | 新疆晶硕新材料有限公司 | Metal oxide and preparation method thereof, preparation facilities |
| CN110354795A (en) * | 2019-05-31 | 2019-10-22 | 广州汇富研究院有限公司 | Gas nozzle, gas reaction equipment and gas hydrolysis method |
| CN111484022A (en) * | 2019-12-23 | 2020-08-04 | 浙江精功新材料技术有限公司 | White carbon black combustion furnace structure |
| CN113817325A (en) * | 2021-11-11 | 2021-12-21 | 陕西省石油化工研究设计院 | Novel high-temperature-resistant flame-retardant silicone rubber and preparation method thereof |
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2009
- 2009-12-28 CN CN200910265416A patent/CN101734668A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001670A (en) * | 2010-10-29 | 2011-04-06 | 沈阳化工股份有限公司 | Method for producing silicon dioxide by using gas phase process |
| CN102001670B (en) * | 2010-10-29 | 2013-04-24 | 沈阳化工股份有限公司 | Method for producing silicon dioxide by using gas phase process |
| CN102476802A (en) * | 2010-11-23 | 2012-05-30 | 北京航天赛德科技发展有限公司 | Preparation method of silica used for leather delustering agent and its device |
| CN102476802B (en) * | 2010-11-23 | 2013-07-10 | 北京航天赛德科技发展有限公司 | Preparation method of silica used for leather delustering agent and its device |
| CN102583396A (en) * | 2012-03-08 | 2012-07-18 | 上海竟茨环保科技有限公司 | Deacidification equipment for producing fumed silica |
| CN102583396B (en) * | 2012-03-08 | 2013-09-25 | 上海竟茨环保科技有限公司 | Deacidification equipment for producing fumed silica |
| CN104628005B (en) * | 2013-11-07 | 2017-08-25 | 浙江开化合成材料有限公司 | A kind of vaporizer, the apparatus and method for producing white carbon |
| CN104628005A (en) * | 2013-11-07 | 2015-05-20 | 浙江开化合成材料有限公司 | Vaporizer, white carbon black production apparatus and white carbon black production method |
| CN106241821A (en) * | 2016-07-21 | 2016-12-21 | 宜昌南玻硅材料有限公司 | The mixing arrangement of a kind of nanoscale fume colloidal silica raw material and method |
| CN106241821B (en) * | 2016-07-21 | 2018-07-03 | 宜昌南玻硅材料有限公司 | A kind of mixing arrangement and method of nanoscale fume colloidal silica raw material |
| CN107777693A (en) * | 2017-11-14 | 2018-03-09 | 宜昌汇富硅材料有限公司 | The production technology and device of a kind of nano fumed silica |
| CN107777693B (en) * | 2017-11-14 | 2021-01-22 | 湖北汇富纳米材料股份有限公司 | Production process and device of nano fumed silica |
| CN108190950A (en) * | 2018-02-06 | 2018-06-22 | 新疆晶硕新材料有限公司 | The preparation method and device of zirconium dioxide |
| CN108585038A (en) * | 2018-04-13 | 2018-09-28 | 新疆晶硕新材料有限公司 | Metal oxide and preparation method thereof, preparation facilities |
| CN110354795A (en) * | 2019-05-31 | 2019-10-22 | 广州汇富研究院有限公司 | Gas nozzle, gas reaction equipment and gas hydrolysis method |
| CN110354795B (en) * | 2019-05-31 | 2020-11-20 | 广州汇富研究院有限公司 | Gas nozzle, gas reaction equipment and gas hydrolysis reaction method |
| CN111484022A (en) * | 2019-12-23 | 2020-08-04 | 浙江精功新材料技术有限公司 | White carbon black combustion furnace structure |
| 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 |
| CN113817325A (en) * | 2021-11-11 | 2021-12-21 | 陕西省石油化工研究设计院 | Novel high-temperature-resistant flame-retardant silicone rubber and preparation method thereof |
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Application publication date: 20100616 |