CN1008085B - Equipment for preparation of paraffin chloride by forced circulating blast method - Google Patents

Abstract

The present invention provides a device for preparing chloroparaffin and other chloride low polymers. In the present invention, chlorine is supplied to the upper part of the non-reaction area of a reaction vessel first, and then the chlorine and hydrogen chloride gas (generated in reaction) are sucked out by a cyclic part; the hydrogen chloride gas is absorbed by water when passing through a jet pump and a liquid storage tank on the cyclic part, residual chlorine is pressed into an agitating device by a cyclic drum, and the purpose of chlorination reaction is achieved; after the reaction, the pressure of the reaction vessel can be pumped by the cyclic part, residual chlorine, and hydrogen chloride gas and water in material are removed to make the material washed by air; then a certain amount of neutralizing and stabilizing agents are thrown in the material, and clean products can be obtained after uniform agitation.

Description

Equipment for preparation of paraffin chloride by forced circulating blast method

The present invention relates to a kind of device of producing the clorafin product.This device also can be used for producing other chloride oligomer product.Below only state with regard to producing clorafin.

Existing Bubbling method device is produced clorafin, and pollution problem is outstanding, and security does not include yet, and investment is bigger.

Task of the present invention provides that a kind of equipment is simple, easy handling, three-waste free pollution, safe and reliable, reduced investment, efficient height, the production equipment with chlorination and two kinds of functions of product postprocessing.

Task of the present invention is finished as follows: whole device is an air-tight state.Mainly form by reaction and circulation two parts and several valves etc.As reactor, wherein three apertures on the kettle cover: put into the chlorine pipe for one, the pipe lower end puts in the still flat with the kettle cover the inside, and the upper end connects chlorine gas source with common glassed steel reaction vessels; An aperture takes on tracheae, the escape pipe lower end on the center line of still chamber, at the bottom of still the distance be still high 1/3.(being as the criterion) not run into reaction mass; An aperture dress is agitated organ pipe, agitates the still bottom of device working portion.Above-described genus reactive moieties; With acid proof pump, squirt pump, stationary tanks etc. are formed cyclic part.The inlet of cyclic part connects the mouth of pipe of giving vent to anger on the still, and its outlet connects agitates the organ pipe mouth.In the device working process, into still internal upper part non-reaction zone is constantly put pure chlorine to the greatest extent by advancing the chlorine pipe in the chlorine source, and cyclic part is constantly chlorine in the still and hydrogen chloride gas (reaction generates) sucking-off.Through squirt pump, stationary tank hydrogenchloride is absorbed by water, and remaining chlorine, cyclic part are constantly compressed into the chlorine drum of remainder again and agitated device, makes the material in the still contact, stir, react with chlorine.Because volume increases behind the water absorbing hydrogen chloride, so increase degree as long as observe the liquid level of stationary tank, the chlorination reaction degree of material as can be known just.Reaction is finished, and can utilize cyclic part that reactor is taken out pressure, makes material obtain air scour, agitate, and obtains cleaner product.

The present invention and existing Bubbling method device relatively have several different places: existing Bubbling method device is by chlorine source pressure bubbling, is to react under bigger pressure, in the hydrogenchloride that reaction generates and discharging.Because the chlorine source directly connects bubbler with pipeline, enter the possibility in chlorine source so exist reactant to flow backwards by pipeline.The present invention only puts into non-reaction zone to pure chlorine, the chlorine source with agitate device not have directly to be connected, to advance the still internal upper part non-reaction zone of chlorine infratubal port, a suitable segment distance is arranged the possibility with regard to not existing the material refluence to enter the chlorine source like this from material.Owing to adopt pump circulation to agitate, can improve the reaction surface of unit time by improving speed of circulation, thereby device can be reacted with fast speeds under normal pressure even under the negative pressure.Obviously, under the prerequisite that does not influence efficient, synthesis under normal pressure is much more superior than compressive reaction.Water in the stationary tank has absorbed hydrogen chloride gas, also has a spot of free chlorine simultaneously, but easily removes, and has removed free chlorine and has just obtained pure most technical hydrochloric acid product.Device can utilize cyclic part that product is carried out aftertreatment in addition, accomplishes that " a tractor serves several purposes " improves the equipment benefit.

Concrete structure of the present invention is provided by following embodiment and schematic flow sheet.

" U " type pipe glass manometer (1).Temperature measurer (2).Chlorine flowrate meter (3).Reactor (4), common glassed steel reaction vessels, 500 liters of volumes.Agitate device (5), can substitute by pvc material, make " " shape, outlet is six ports of horizontal arm below.Enamel cover (6), in lay temperature measurer probe.Needle type valve (7), the chlorine flowrate in control chlorine source.Advance chlorine pipe (8).Agitate organ pipe (9).Escape pipe (10).Valve (11), an end is logical agitates organ pipe, and an end leads to atmosphere.Valve (12), the outlet of agitating organ pipe mouth and cyclic part of reactive moieties cuts off switch." U " U-tube manometer (13); respectively there is the glass envelope of 0.5 liter of a volume at two ends; when the pressure on being added in " U " type pipe is excessive like this; liquid in the pipe can be ensconced in the bubble; after excessive pressure is eliminated; liquid in the bubble can return in the pipe again automatically, and this has in fact also played a kind of self-balancing pressure, can protect stationary tank.Liquidometer (14), glass material, on be carved with scale.The outlet of cyclic part (15).Valve (16) can be regulated the circulation ability of cyclic part, thus reaction speed open, it is slack-off to circulate, otherwise fast.Squirt pump (17), pvc material is welded into, with the acid proof pump power match.Stationary tank (18), pvc material is welded into, and 200 liters of volumes, right cylinder, diameter are high by 1/3, cooling tube (19), plastic hose, 2 centimetres of pipe diameters, 2 square metres of total surface areas are used for cooling off stationary tank.Acid proof pump (20), 3 kilowatts of power.The inlet of cyclic part (21), valve (22), an end connects on the cyclic part outlet pipe, and an end leads to the alkali groove.Reaction mass (23).Connecting tube can adopt 2 inches polyvinyl chloride hard tubes substantially.

Operating process is as follows: building in refining solid wax or the liquid wax input still, stop after being heated to 80 ℃, drive valve (7) and put pure chlorine into, close valve (12), close valve (11), drive valve (22), starter motor squirt pump work simultaneously, clean the air displacement in the still, after the air in the still changes only, drive valve (12), close valve (22) and carry out normal reaction, in the reasonable time of the reaction after, because the water in the stationary tank has absorbed hydrogen chloride gas, liquid level raises, and liquid level is elevated to certain height, promptly shows to react to finish.Because be reacted to latter stage, material in the still can be more and more sticking, pressure difference between stationary tank (18) and the reactor (4) can increase, so change as long as observe " U " type (13) liquid level difference, also can release the reaction degree of carrying out, the speed of response speed can be by closing, driving valve (16) and regulate, it is fast to fasten valve (16) reaction, otherwise slow.Temperature of reaction is controlled between 80 ℃-100 ℃, and too high as temperature, chlorine dose is advanced in available minimizing, fetches water toward the still chuck, reduces measure coolings such as speed of circulation.Reaction is finished, the reacting kettle jacketing cooling is gone in water flowing, make material be cooled to 75 ℃, and maintain, turn off the chlorine source then, dead " U " type meter (1) of gambling is gone up pipeline with " U " type meter (13), turn off (12), drive valve (22), cyclic part works on, and remaining chlorine in the still and hydrogen chloride gas are extracted out, send into the neutralization of alkali groove, after being extracted into certain vacuum in the still, open valve (11), allow air constantly by agitating device to enter in the still, make material obtain the flushing of air, when being flushed to a certain degree, again by above way, the pass is opened corresponding valve and is vacuumized ...Behind the several, just removed remaining chlorine, hydrogen chloride gas and moisture content in the interior material of still so repeatedly.Drop into a certain amount of neutralizing agent and stablizer then, agitate evenly again after, promptly obtain cleaner clorafin product.Also obtain the technical hydrochloric acid of byproduct concentration 30% simultaneously.

Claims (1)

1. A kind of pump circulation method of agitating is produced the method for oxidized petroleum wax, it comprises sends into non-reaction zone space, reactor top with chlorine through advancing the chlorine pipe, the hydrogen chloride gas that chlorine in the still and reaction generate is extracted out through the mouth of pipe of giving vent to anger that is positioned at still chamber center line, the gas of being extracted out enters stationary tank through squirt pump, hydrogen chloride gas is absorbed by water in squirt pump and stationary tank, the chlorine drum of remainder is compressed into the device of agitating that is positioned at the reactor bottom, so continuously, the interior material of chlorine and still is fully contacted and rapid reaction fast.

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