CN104016713A - High-temperature-resistance dipping method for hydrogen chloride synthetic furnace graphite combustion chamber - Google Patents

High-temperature-resistance dipping method for hydrogen chloride synthetic furnace graphite combustion chamber Download PDF

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CN104016713A
CN104016713A CN201410219640.1A CN201410219640A CN104016713A CN 104016713 A CN104016713 A CN 104016713A CN 201410219640 A CN201410219640 A CN 201410219640A CN 104016713 A CN104016713 A CN 104016713A
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hydrogen chloride
synthetic furnace
chloride synthetic
burning chamber
hours
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CN104016713B (en
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潘东海
潘越
赵小明
刘丹丹
唐亚军
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Abstract

The invention discloses a high-temperature-resistance dipping method for a hydrogen chloride synthetic furnace graphite combustion chamber, which is characterized in that the hydrogen chloride synthetic furnace graphite combustion chamber is subjected to high-temperature-resistance dipping by a polysiloxane organosilicon water-soluble dispersion liquid, the hydrogen chloride synthetic furnace graphite combustion chamber product is dipped, solidified and performed heat drying step by step, the antioxidation performance of the hydrogen chloride synthetic furnace graphite combustion chamber product under a high temperature state is increased, mechanical strength and corrosion resisting stability of the graphite combustion chamber product are enhanced, and the usage life of the hydrogen chloride synthetic furnace graphite combustion chamber is prolonged.

Description

A kind of hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process
Technical field:
Patent of the present invention relates to a kind of hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process.
Background technology:
Hydrogen chloride synthetic furnace graphite burning chamber is the key part of hydrogen chloride synthetic furnace.Adopt at present the byproduct steam hydrogen chloride synthetic furnace of graphite-steel-graphite-structure both at home and abroad, the most resol that adopts of graphite burning chamber goods of its synthetic furnace hypomere carries out dip treating, but high-temperature resistant result is undesirable, in use easily cause the problem of graphite explosion.Have recently and adopt tetrafluoroethylene graphite product to be carried out to the research report of fire-resistant oxidation resistant dip treating, but because tetrafluoroethylene and graphite body do not have good binding property, macerate is easily separated out, practical effect is undesirable.Therefore, the fire-resistant oxidation resistant performance of hydrogen chloride synthetic furnace graphite burning chamber, is all subject to certain restrictions synthetic continuous operation and security, the practicality of producing of hydrogenchloride.
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 chamber high temperature resisting dipping treatment process, further improve resistance to elevated temperatures master's antioxidant property under the condition of high temperature of hydrogen chloride synthetic furnace graphite burning chamber graphite product, make the longer service life of hydrogen chloride synthetic furnace graphite burning chamber of a specified duration, meet the requirement of the synthetic continuous production operation of hydrogenchloride and security, practicality.
The technical solution of patent of the present invention is:
For hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping, process the problem existing in production practice, described in patent of the present invention, hydrogen chloride synthetic furnace graphite burning chamber adopts polysiloxane organic silicon water soluble dispersion liquid to carry out high temperature resisting dipping processing, hydrogen chloride synthetic furnace graphite burning chamber goods are through step impregnation, solidify and the operation process such as heated drying processing, in the surface of graphite product and hole, produce stable anti-oxidant phase, improve the antioxidant effect of graphite product, solve the difficult problem that in graphite material processing, macerate adhesion amount is few and the degree of depth is inhomogeneous, improve the antioxidant property of hydrogen chloride synthetic furnace graphite burning chamber goods under the condition of high temperature, strengthen physical strength and the corrosion-resistant stability of graphite burning chamber goods, extend the work-ing life of hydrogen chloride synthetic furnace graphite burning chamber.
A kind of hydrogen chloride synthetic furnace graphite burning of the present invention chamber high temperature resisting dipping treatment process, to adopt polysiloxane organosilicon to carry out high temperature resisting dipping processing to hydrogen chloride synthetic furnace graphite burning chamber goods, its process program is: first prepare the hexamethyldisiloxane of 36-42% mass percent and the water-soluble dispersion liquid of polydimethylsiloxane of 0.06-8% mass percent is steeping fluid, steeping fluid is joined and in impregnating autoclave, is warmed to 50-85 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into again 0.6-0.9Mpa, keep dipping 4-6 hour, so repeatedly after 2-3 time, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, heat-up rate with 5-15 ℃/h, through 28-42 hour, by room temperature, being warmed up to gradually 320 ℃ is cured and drying treatment, make the graphite burning chamber goods of dipping fully solidify and be dried, complete the dip treating technique of hydrogen chloride synthetic furnace graphite burning chamber goods, obtain having the hydrogen chloride synthetic furnace graphite burning chamber goods of better resistance to elevated temperatures.
Described employing polysiloxane organosilicon carries out high temperature resisting dipping treatment process to hydrogen chloride synthetic furnace graphite burning chamber goods, also comprise that adopting 38-42% cyclohexyl methyl siloxanes and the water-soluble dispersion liquid of 0.08-8% polydimethylsiloxane is steeping fluid, steeping fluid is joined and in impregnating autoclave, is warmed to 50-85 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into again 0.6-0.9Mpa, keep dipping 4-6 hour, so repeatedly after 2-3 time, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, heat-up rate with 5-15 ℃/h, through 28-42 hour, by room temperature, being warmed up to gradually 320 ℃ is cured and drying treatment, make the graphite burning chamber goods of dipping fully solidify and be dried, complete the dip treating technique of hydrogen chloride synthetic furnace graphite burning chamber goods, obtain having the hydrogen chloride synthetic furnace graphite burning chamber goods of better resistance to elevated temperatures.
The process program of described a kind of hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process, that employing 38% hexamethyldisiloxane and the water-soluble dispersion liquid of 0.08% polydimethylsiloxane are steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 65 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 480mmHg, keep dipping 2 hours, be forced into again 0.7Mpa, keep dipping 6 hours, so repeatedly after 3 times, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, first at room temperature dry 3 hours, then the heat-up rate with 9 ℃/h is dried 9 hours 80-160 ℃ of temperature range, heat-up rate with 6 ℃/h is dried 18 hours 170-280 ℃ of temperature range again, heat-up rate with 5 ℃/h is dried 6 hours 290-320 ℃ of temperature range, make the graphite burning chamber goods of dipping fully solidify and be dried, complete the dip treating technique of hydrogen chloride synthetic furnace graphite burning chamber goods, obtain having the hydrogen chloride synthetic furnace graphite burning chamber goods of better resistance to elevated temperatures.
The process program of described a kind of hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process, also comprise that adopting 40% cyclohexyl methyl siloxanes and the water-soluble dispersion liquid of 0.08% polydimethylsiloxane is steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 70 ℃, then graphite product is placed in to impregnating autoclave, be evacuated down to 460mmHg, keep dipping 2 hours, be forced into again 0.7Mpa, keep dipping 6 hours, so repeatedly after 2 times, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, first at room temperature dry 3 hours, then the heat-up rate with 8 ℃/h is dried 10 hours 80-160 ℃ of temperature range, heat-up rate 170-280 ℃ temperature range with 5.5 ℃/h is dried 20 hours again, heat-up rate with 5 ℃/h is dried 6 hours 290-320 ℃ of temperature range, make the graphite burning chamber goods of dipping fully solidify and be dried, complete the dip treating technique of hydrogen chloride synthetic furnace graphite product, obtain having the hydrogen chloride synthetic furnace graphite burning chamber goods of better resistance to elevated temperatures.
Embodiment:
Embodiment mono-: the process program of a kind of hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process is to choose that apparent porosity is 14%, volume density is 1700kg/cm 3graphite material make hydrogen chloride synthetic furnace graphite burning chamber goods, adopting 38% hexamethyldisiloxane and the water-soluble dispersion liquid of 0.08% polydimethylsiloxane is steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 65 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 480mmHg, keep dipping 2 hours, be forced into again 0.7Mpa, keep dipping 6 hours, so repeatedly after 3 times, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, first at room temperature dry 3 hours, then the heat-up rate with 9 ℃/h is dried 9 hours 80-160 ℃ of temperature range, heat-up rate with 6 ℃/h is dried 18 hours 170-280 ℃ of temperature range again, heat-up rate with 5 ℃/h is dried 6 hours 290-320 ℃ of temperature range, make the graphite burning chamber goods of dipping fully solidify and be dried, complete the dip treating technique of hydrogen chloride synthetic furnace graphite product, obtain having the hydrogen chloride synthetic furnace graphite burning chamber goods of better resistance to elevated temperatures.
Embodiment bis-: the process program of a kind of hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process is to choose that apparent porosity is 15%, volume density is 1800kg/cm 3graphite material make hydrogen chloride synthetic furnace graphite burning chamber goods, adopting 40% cyclohexyl methyl siloxanes and the water-soluble dispersion liquid of 0.08% polydimethylsiloxane is steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 70 ℃, then graphite product is placed in to impregnating autoclave, be evacuated down to 460mmHg, keep dipping 2 hours, be forced into again 0.7Mpa, keep dipping 6 hours, so repeatedly after 2 times, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, first at room temperature dry 3 hours, then the heat-up rate with 8 ℃/h is dried 10 hours 80-160 ℃ of temperature range, heat-up rate 170-280 ℃ temperature range with 5.5 ℃/h is dried 20 hours again, heat-up rate with 5 ℃/h is dried 6 hours 290-320 ℃ of temperature range, make the graphite burning chamber goods of dipping fully solidify and be dried, complete the dip treating technique of hydrogen chloride synthetic furnace graphite product, obtain having the hydrogen chloride synthetic furnace graphite burning chamber goods of better resistance to elevated temperatures.

Claims (5)

1. a hydrogen chloride synthetic furnace graphite burning chamber high temperature resisting dipping treatment process, is characterized in that: hydrogen chloride synthetic furnace graphite burning chamber adopts polysiloxane organic silicon water soluble dispersion liquid to carry out high temperature resisting dipping processing.
2. a kind of hydrogen chloride synthetic furnace graphite burning according to claim 1 chamber high temperature resisting dipping treatment process, it is characterized in that: adopting 36-42% hexamethyldisiloxane and the water-soluble dispersion liquid of 0.06-8% polydimethylsiloxane is steeping fluid, steeping fluid is joined and in impregnating autoclave, is warmed to 50-85 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into again 0.6-0.9Mpa, keep dipping 4-6 hour, so repeatedly after 2-3 time, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, heat-up rate with 5-15 ℃/h, through 28-42 hour, by room temperature, being warmed up to gradually 320 ℃ is cured and drying treatment, complete the dip treating technique of hydrogen chloride synthetic furnace graphite burning chamber goods.
3. a kind of hydrogen chloride synthetic furnace graphite burning according to claim 1 chamber high temperature resisting dipping treatment process, it is characterized in that: adopting 38-42% cyclohexyl methyl siloxanes and the water-soluble dispersion liquid of 0.08-8% polydimethylsiloxane is steeping fluid, steeping fluid is joined and in impregnating autoclave, is warmed to 50-85 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 460-580mmHg, keep dipping 1.6-2.4 hour, be forced into again 0.6-0.9Mpa, keep dipping 4-6 hour, so repeatedly after 2-3 time, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, heat-up rate with 5-15 ℃/h, through 28-42 hour, by room temperature, being warmed up to gradually 320 ℃ is cured and drying treatment, complete the dip treating technique of hydrogen chloride synthetic furnace graphite burning chamber goods.
4. a kind of hydrogen chloride synthetic furnace graphite burning according to claim 2 chamber high temperature resisting dipping treatment process, is characterized in that: choose apparent porosity and be 14%, volume density is 1700kg/cm 3graphite material make hydrogen chloride synthetic furnace graphite burning chamber goods, adopting 38% hexamethyldisiloxane and the water-soluble dispersion liquid of 0.08% polydimethylsiloxane is steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 65 ℃, graphite burning chamber goods are placed in to impregnating autoclave, be evacuated down to 480mmHg, keep dipping 2 hours, be forced into again 0.7Mpa, keep dipping 6 hours, so repeatedly after 3 times, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, first at room temperature dry 3 hours, then the heat-up rate with 9 ℃/h is dried 9 hours 80-160 ℃ of temperature range, heat-up rate with 6 ℃/h is dried 18 hours 170-280 ℃ of temperature range again, heat-up rate with 5 ℃/h is dried 6 hours 290-320 ℃ of temperature range, complete the dip treating technique of hydrogen chloride synthetic furnace graphite burning chamber goods.
5. a kind of hydrogen chloride synthetic furnace graphite burning according to claim 3 chamber high temperature resisting dipping treatment process, is characterized in that: choose apparent porosity and be 15%, volume density is 1800kg/cm 3graphite material make hydrogen chloride synthetic furnace graphite burning chamber goods, adopting 40% cyclohexyl methyl siloxanes and the water-soluble dispersion liquid of 0.08% polydimethylsiloxane is steeping fluid, steeping fluid is joined in impregnating autoclave and is warmed to 70 ℃, then graphite product is placed in to impregnating autoclave, be evacuated down to 460mmHg, keep dipping 2 hours, be forced into again 0.7Mpa, keep dipping 6 hours, so repeatedly after 2 times, in steeping fluid by graphite burning chamber goods from impregnating autoclave, take out, first at room temperature dry 3 hours, then the heat-up rate with 8 ℃/h is dried 10 hours 80-160 ℃ of temperature range, heat-up rate 170-280 ℃ temperature range with 5.5 ℃/h is dried 20 hours again, heat-up rate with 5 ℃/h is dried 6 hours 290-320 ℃ of temperature range, complete the dip treating technique of hydrogen chloride synthetic furnace graphite product.
CN201410219640.1A 2014-05-20 2014-05-20 A kind of hydrogen chloride synthetic furnace graphite burning room high temperature resisting dipping treatment process Expired - Fee Related CN104016713B (en)

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JPS6220534A (en) * 1985-07-19 1987-01-29 Showa Electric Wire & Cable Co Ltd Heat-resistant prepreg
US6787189B2 (en) * 2001-12-03 2004-09-07 Shin-Etsu Chemical Co., Ltd. Preparation of C/Si/O composite material
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