CN104016713B - A kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process - Google Patents
A kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process Download PDFInfo
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- CN104016713B CN104016713B CN201410219640.1A CN201410219640A CN104016713B CN 104016713 B CN104016713 B CN 104016713B CN 201410219640 A CN201410219640 A CN 201410219640A CN 104016713 B CN104016713 B CN 104016713B
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- hydrogen chloride
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- chloride synthetic
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Abstract
The present invention patent discloses a kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process, it is characterized in that: hydrogen chloride synthetic furnace graphite burning room adopts polysiloxane organic silicon water soluble dispersion liquid to carry out high temperature resisting dipping process, hydrogen chloride synthetic furnace graphite burning room goods are through process such as step impregnation, solidification and heated drying process, improve hydrogen chloride synthetic furnace graphite burning room goods antioxidant property at high operating temperatures, strengthen the physical strength of graphite burning room goods and corrosion-resistant stability, extend the work-ing life of hydrogen chloride synthetic furnace graphite burning room.
Description
Technical field:
Patent of the present invention relates to a kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process.
Background technology:
Hydrogen chloride synthetic furnace graphite burning room is the key part of hydrogen chloride synthetic furnace.Adopt the byproduct steam hydrogen chloride synthetic furnace of graphite-steel-graphite-structure at present both at home and abroad, the graphite burning room goods majority of its synthetic furnace hypomere adopts resol to carry out dip treating, but high-temperature resistant result is undesirable, in use easily cause the problem that graphite bursts.Have recently and adopt tetrafluoroethylene to carry out the research report of fire-resistant oxidation resistant dip treating to graphite product, but do not have good binding property due to tetrafluoroethylene and graphite body, macerate is easily separated out, and practical effect is undesirable.Therefore, the fire-resistant oxidation resistant performance of hydrogen chloride synthetic furnace graphite burning room, the continuous operation that hydrogen chloride synthesis is produced and security, practicality are all subject to certain restrictions.
Summary of the invention:
The object of patent of the present invention is to provide a kind of brand-new hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process, the resistance to elevated temperatures master antioxidant property at high operating temperatures of further raising hydrogen chloride synthetic furnace graphite burning room graphite product, make the longer service life of hydrogen chloride synthetic furnace graphite burning room of a specified duration, meet hydrogen chloride synthesis continuous production run and security, practicality requirement.
The technical solution of patent of the present invention is:
For hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping process Problems existing in production practice, hydrogen chloride synthetic furnace graphite burning room described in patent of the present invention adopts polysiloxane organic silicon water soluble dispersion liquid to carry out high temperature resisting dipping process, hydrogen chloride synthetic furnace graphite burning room goods are through step impregnation, the process such as solidification and heated drying process, stable anti-oxidant phase is produced in the surface and hole of graphite product, improve the antioxidant effect of graphite product, solve the few and difficult problem that the degree of depth is uneven of macerate adhesion amount in graphite material process, improve hydrogen chloride synthetic furnace graphite burning room goods antioxidant property at high operating temperatures, strengthen the physical strength of graphite burning room goods and corrosion-resistant stability, extend the work-ing life of hydrogen chloride synthetic furnace graphite burning room.
A kind of hydrogen chloride synthetic furnace graphite burning room of the present invention high temperature resisting dipping treatment process, adopt polysiloxane organosilicon to carry out high temperature resisting dipping process to hydrogen chloride synthetic furnace graphite burning room goods, its process program is: first the hexamethyldisiloxane of preparation 36-42% mass percent and the polydimethylsiloxane aqueous dispersion of 0.06-8% mass percent are steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 50-85 DEG C, graphite burning room goods are placed in impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into 0.6-0.9Mpa again, keep dipping 4-6 hour, so repeatedly after 2-3 time, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, with the heat-up rate of 5-15 DEG C/h, be warmed up to 320 DEG C through 28-42 hour gradually by room temperature to be cured and drying treatment, the graphite burning room goods of dipping are fully solidified and drying, namely the dip treating technique of hydrogen chloride synthetic furnace graphite burning room goods is completed, obtain the hydrogen chloride synthetic furnace graphite burning room goods with better resistance to elevated temperatures.
Described employing polysiloxane organosilicon carries out high temperature resisting dipping treatment process to hydrogen chloride synthetic furnace graphite burning room goods, also comprise and adopt 38-42% cyclomethicone and 0.08-8% polydimethylsiloxane aqueous dispersion to be steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 50-85 DEG C, graphite burning room goods are placed in impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into 0.6-0.9Mpa again, keep dipping 4-6 hour, so repeatedly after 2-3 time, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, with the heat-up rate of 5-15 DEG C/h, be warmed up to 320 DEG C through 28-42 hour gradually by room temperature to be cured and drying treatment, the graphite burning room goods of dipping are fully solidified and drying, namely the dip treating technique of hydrogen chloride synthetic furnace graphite burning room goods is completed, obtain the hydrogen chloride synthetic furnace graphite burning room goods with better resistance to elevated temperatures.
The process program of described a kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process, be employing 38% hexamethyldisiloxane and 0.08% polydimethylsiloxane aqueous dispersion be steeping fluid, steeping fluid is joined in impregnating autoclave and be warmed to 65 DEG C, graphite burning room goods are placed in impregnating autoclave, be evacuated down to 480mmHg, keep dipping 2 hours, be forced into 0.7Mpa again, keep dipping 6 hours, so repeatedly after 3 times, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, first at room temperature dry 3 hours, then with the heat-up rate of 9 DEG C/h dry 9 hours of 80-160 DEG C of temperature range, again with the heat-up rate of 6 DEG C/h dry 18 hours of 170-280 DEG C of temperature range, with the heat-up rate of 5 DEG C/h 290-320 DEG C of temperature range drying 6 hours, the graphite burning room goods of dipping are fully solidified and drying, namely the dip treating technique of hydrogen chloride synthetic furnace graphite burning room goods is completed, obtain the hydrogen chloride synthetic furnace graphite burning room goods with better resistance to elevated temperatures.
The process program of described a kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process, also comprise employing 40% cyclomethicone and 0.08% polydimethylsiloxane aqueous dispersion is steeping fluid, steeping fluid is joined in impregnating autoclave and be warmed to 70 DEG C, then graphite product is placed in impregnating autoclave, be evacuated down to 460mmHg, keep dipping 2 hours, be forced into 0.7Mpa again, keep dipping 6 hours, so repeatedly after 2 times, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, first at room temperature dry 3 hours, then with the heat-up rate of 8 DEG C/h dry 10 hours of 80-160 DEG C of temperature range, again with the heat-up rate 170-280 of 5.5 DEG C/h DEG C of temperature range drying 20 hours, with the heat-up rate of 5 DEG C/h 290-320 DEG C of temperature range drying 6 hours, the graphite burning room goods of dipping are fully solidified and drying, namely the dip treating technique of hydrogen chloride synthetic furnace graphite product is completed, obtain the hydrogen chloride synthetic furnace graphite burning room goods with better resistance to elevated temperatures.
Embodiment:
Embodiment one: the process program of a kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process chooses that apparent porosity is 14%, volume density is 1700kg/cm
3graphite material make hydrogen chloride synthetic furnace graphite burning room goods, 38% hexamethyldisiloxane and 0.08% polydimethylsiloxane aqueous dispersion is adopted to be steeping fluid, steeping fluid is joined in impregnating autoclave and be warmed to 65 DEG C, graphite burning room goods are placed in impregnating autoclave, be evacuated down to 480mmHg, keep dipping 2 hours, be forced into 0.7Mpa again, keep dipping 6 hours, so repeatedly after 3 times, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, first at room temperature dry 3 hours, then with the heat-up rate of 9 DEG C/h dry 9 hours of 80-160 DEG C of temperature range, again with the heat-up rate of 6 DEG C/h dry 18 hours of 170-280 DEG C of temperature range, with the heat-up rate of 5 DEG C/h 290-320 DEG C of temperature range drying 6 hours, the graphite burning room goods of dipping are fully solidified and drying, namely the dip treating technique of hydrogen chloride synthetic furnace graphite product is completed, obtain the hydrogen chloride synthetic furnace graphite burning room goods with better resistance to elevated temperatures.
Embodiment two: the process program of a kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process chooses that apparent porosity is 15%, volume density is 1800kg/cm
3graphite material make hydrogen chloride synthetic furnace graphite burning room goods, 40% cyclomethicone and 0.08% polydimethylsiloxane aqueous dispersion is adopted to be steeping fluid, steeping fluid is joined in impregnating autoclave and be warmed to 70 DEG C, then graphite product is placed in impregnating autoclave, be evacuated down to 460mmHg, keep dipping 2 hours, be forced into 0.7Mpa again, keep dipping 6 hours, so repeatedly after 2 times, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, first at room temperature dry 3 hours, then with the heat-up rate of 8 DEG C/h dry 10 hours of 80-160 DEG C of temperature range, again with the heat-up rate 170-280 of 5.5 DEG C/h DEG C of temperature range drying 20 hours, with the heat-up rate of 5 DEG C/h 290-320 DEG C of temperature range drying 6 hours, the graphite burning room goods of dipping are fully solidified and drying, namely the dip treating technique of hydrogen chloride synthetic furnace graphite product is completed, obtain the hydrogen chloride synthetic furnace graphite burning room goods with better resistance to elevated temperatures.
Claims (2)
1. a hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process, it is characterized in that: adopt the hexamethyldisiloxane of 36-42% mass percent and the polydimethylsiloxane aqueous dispersion of 0.06-8% mass percent to be steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 50-85 DEG C, graphite burning room goods are placed in impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into 0.6-0.9Mpa again, keep dipping 4-6 hour, so repeatedly after 2-3 time, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, with the heat-up rate of 5-15 DEG C/h, be warmed up to 320 DEG C through 28-42 hour gradually by room temperature to be cured and drying treatment, namely the dip treating technique of hydrogen chloride synthetic furnace graphite burning room goods is completed.
2. a kind of hydrogen chloride synthetic furnace graphite burning room according to claim 1 high temperature resisting dipping treatment process, is characterized in that: choose that apparent porosity is 14%, volume density is 1700kg/cm
3graphite material make hydrogen chloride synthetic furnace graphite burning room goods, the hexamethyldisiloxane of 38% mass percent and the polydimethylsiloxane aqueous dispersion of 0.08% mass percent is adopted to be steeping fluid, steeping fluid is joined in impregnating autoclave and be warmed to 65 DEG C, graphite burning room goods are placed in impregnating autoclave, be evacuated down to 480mmHg, keep dipping 2 hours, be forced into 0.7Mpa again, keep dipping 6 hours, so repeatedly after 3 times, graphite burning room goods are taken out in the steeping fluid impregnating autoclave, first at room temperature dry 3 hours, then with the heat-up rate of 9 DEG C/h dry 9 hours of 80-160 DEG C of temperature range, again with the heat-up rate of 6 DEG C/h dry 18 hours of 170-280 DEG C of temperature range, with the heat-up rate of 5 DEG C/h 290-320 DEG C of temperature range drying 6 hours, namely the dip treating technique of hydrogen chloride synthetic furnace graphite burning room goods is completed.
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| JPH0645709B2 (en) * | 1985-07-19 | 1994-06-15 | 昭和電線電纜株式会社 | Method for manufacturing heat resistant prepreg |
| JP2003171180A (en) * | 2001-12-03 | 2003-06-17 | Shin Etsu Chem Co Ltd | METHOD FOR MANUFACTURING C/Si/O COMPOSITE MATERIAL |
| US20030209610A1 (en) * | 2001-12-14 | 2003-11-13 | Edward Miller | High velocity oxygen fuel (HVOF) method for spray coating non-melting polymers |
| CN1317238C (en) * | 2004-09-24 | 2007-05-23 | 中国人民解放军国防科学技术大学 | Method for preparing composite rail control thrust chamber by pioneer impregnating cracking technology |
| FR2986228B1 (en) * | 2012-01-31 | 2014-02-28 | Commissariat Energie Atomique | CREUSET FOR SOLIDIFICATION OF SILICON INGOT. |
| CN103708846B (en) * | 2013-12-27 | 2014-11-05 | 湖南中坚科技有限公司 | Preparation method of C/C-SiC composite material |
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