CN101838542A - Manufacturing method of ultra-temperature pitch - Google Patents

Abstract

The invention relates to a manufacturing method of ultra-temperature pitch using coal pitch as a raw material, comprising the following steps of: a, evenly heating a medium-temperature liquid coal pitch raw material insulated at the temperature of 180 DEG C at the speed of 13-15 DEG C per hour and mixing by starting a mixing device when the temperature raises to 250 DEG C in a kettle; b, carrying out oxidation reaction when the temperature raises to 320 DEG C in the kettle and carrying out reduced pressure distillation after the distillate quantity is stable; c, when the temperature raises to 375+/-5 DEG C, stopping raising the temperature, maintaining the temperature, sampling, analyzing softening points until the softening points satisfy product requirements, wherein the total oxidation reaction time reaches 5-10 hours; stopping heating, introducing air and evacuating, discharging, and cooling to the normal temperature. The manufacturing method of ultra-temperature pitch can not cause local overheating concentration, leads aggregated molecules to have even distribution and stable quality, can produce high-temperature and ultra-temperature pitch according to requirements, shortens the production time, prolongs the service life of a device, and greatly improves the product quality.

Description

The manufacture method of ultra-temperature pitch

Technical field

The present invention relates to a kind of is the manufacture method of the ultra-temperature pitch of raw material with the coal-tar pitch.

Background technology

The coal-tar pitch raw material can produce the asphaltic products. of the mass parameter of different qualities by follow-up distillation treatment process, and the purposes difference according to asphaltic products. also is not quite similar to the bituminous parameter request, and wherein the bituminous softening temperature is its key property parameter.Existing asphalt production process mainly contains methods such as horizontal retort intermittent type atmospheric distillation, the continuous atmospheric distillation of tube furnace, horizontal retort decompression single flash method, these traditional technologys are mainly used in produces lower middle temperature, the modified pitch of softening temperature, the product softening temperature can only reach 120 ℃ at most usually, if produce the higher pitch of softening temperature, defective such as these production technique just exist that the easy coking of Distallation systm equipment, obstruction, equipment are fragile, unstable product quality, asphaltic products. molecular distribution are difficult for evenly, need frequent clear still, seriously polluted.If produce the ultra-temperature pitch product of 170 ℃～320 ℃ of softening temperatures, then traditional production technique is difficult to realize.

Summary of the invention

Technical problem to be solved by this invention is, a kind of manufacture method that can produce high-quality, high softening-point and the uniform ultra-temperature pitch of molecular distribution is provided.

The manufacture method of ultra-temperature pitch of the present invention is passed through following steps successively:

A. will be incubated at 180 ℃ middle temperature liquid coal asphalt stock and send into upright still, start electrical heating device, evenly heat up, and open whipping device when temperature in the kettle rises to 250 ℃ and stir with per hour 13 ℃～15 ℃ speed by the insulation delivery system;

B. when temperature in the kettle rises to 320 ℃, open compressed air inlet valve, with per minute 1M ³The pressurized air of flow by pipeline even air inlet at the bottom of the still, make oxidizing reaction, treat that quantity of distillate carries out underpressure distillation after stable, the flow that vacuum pump vacuumizes during underpressure distillation is per minute 6～8M ³, the vacuum meter registration is not less than 0.9MPa;

C. when temperature in the kettle rises to 375 ± 5 ℃, stop to heat up and keeping temperature, begin to take a sample and the softening temperature analysis, satisfy product requirement and total oxidation time reaches 5～10 hours until softening temperature, stop heating, stop air inlet, stop to vacuumize, open bleeder valve at the bottom of the still, close the distillation outlet, feed compressed nitrogen, finished product pitch is pressed into receiver is cooled to normal temperature.

The present invention adopts vertical mechanical to stir, automatically controlledly adds thermal still, utilizes compressed air oxidation and stir, adopt vacuum distillation method simultaneously, material is reduced pressure at high temperature, and card fully obtains stirring, the still wall is heated evenly, reacts completely, can not cause the local superheating coking, make the polymeric molecular distribution evenly, steady quality, can produce the high temperature ultra-temperature pitch as requested, the bituminous softening temperature reaches as high as 320 ℃; In addition owing to adopt machinery and pressurized air to stir and underpressure distillation, shortened the production time greatly, temperature in the kettle also can reduce about 20 ℃, prolong the work-ing life of equipment effectively, increased substantially quality product, can provide reliable hard pitch base mateiral for high-end products such as asphalt base carbon fibers.

Embodiment

The making method of embodiment of the invention system passes through following steps successively:

A. will be incubated at 180 ℃ middle temperature liquid coal asphalt stock and send into 13M by the insulation delivery system ³Upright still, advance real 12 tons, start electrical heating device, evenly heat up with 14 ℃ speed per hour, open whipping device when temperature in the kettle rises to 250 ℃ and stir;

B. when temperature in the kettle rises to 320 ℃, open compressed air inlet valve, with per minute 1M ³The pressurized air of flow by pipeline even air inlet at the bottom of the still, make oxidizing reaction, treat that quantity of distillate carries out underpressure distillation after stable, the flow that vacuum pump vacuumizes during underpressure distillation is per minute 8M ³, the vacuum meter registration is not less than 0.9MPa;

C. when temperature in the kettle rises to 375 ± 5 ℃, stop to heat up and keeping temperature, begin to take a sample and the softening temperature analysis, satisfy product requirement and total oxidation time is not less than 8 hours until softening temperature, stop heating, stop air inlet, stop to vacuumize, open bleeder valve at the bottom of the still, close the distillation outlet, feed compressed nitrogen, finished product pitch is pressed into receiver is cooled to normal temperature, packing, warehouse-in.

The asphaltic products. of 250 ℃ of softening temperatures that the embodiment of the invention is produced and 115 ℃, the asphaltic products. of its every index and traditional technology production is compared as follows:

Above data as can be seen, method of the present invention not only can be produced high-end product, even be used to produce 115 ℃ of character asphaltic products.es, its quality product also is better than the product that traditional technology is produced.

Claims (1)

1. the manufacture method of a ultra-temperature pitch is characterized in that: pass through following steps successively,

A. will be incubated at 180 ℃ middle temperature liquid coal asphalt stock and send into upright still, start electrical heating device, evenly heat up, and open whipping device when temperature in the kettle rises to 250 ℃ and stir with per hour 13 ℃～15 ℃ speed by the insulation delivery system;

B. when temperature in the kettle rises to 320 ℃, open compressed air inlet valve, with per minute 1M ³The pressurized air of flow by pipeline even air inlet at the bottom of the still, make oxidizing reaction, treat that quantity of distillate carries out underpressure distillation after stable, the flow that vacuum pump vacuumizes during underpressure distillation is per minute 6～8M ³, the vacuum meter registration is not less than 0.9MPa;

C. when temperature in the kettle rises to 375 ± 5 ℃, stop to heat up and keeping temperature, begin to take a sample and the softening temperature analysis, satisfy product requirement and total oxidation time reaches 5～10 hours until softening temperature, stop heating, stop air inlet, stop to vacuumize, open bleeder valve at the bottom of the still, close the distillation outlet, feed compressed nitrogen, finished product pitch is pressed into receiver is cooled to normal temperature.