CN101774579A - Recovery of CS in insoluble sulphur production2Method (2) - Google Patents

Abstract

The invention discloses a method for recovering CS in the production process of insoluble sulfur₂The method comprises the following specific operations: 1. firstly, adding 1.8-2.2 t of CS into a distillation kettle₂Opening a small spiral tube steam valve of the mother liquor, controlling the pressure to be 0.14-0.16 MPa, and adding the mother liquor at the flow rate of 1.4-1.6 t/h for 28-32 t after the gas phase temperature reaches 46-50 ℃; 2. after the mother liquor feeding is finished, raising the gas phase temperature to be higher than 50 ℃, opening a large spiral pipe steam valve, heating for 100-140 min under the pressure of 0.4-0.5 MPa; 3. when the temperature in the kettle reaches 130-140 ℃, opening a straight-through pipe steam valve inserted into the bottom, heating for 14-18 min under the pressure of 0.3-0.5 MPa, and when the gas phase temperature rises to 90-95 ℃, ending distillation, and recovering CS from a condenser through a recovery pipe at the top of the tower₂. The invention adopts micro-positive pressure and water vapor extraction azeotropic distillation to recover CS₂New process, improved CS₂Boiling point of the refrigerant in the condenser to the CS₂The temperature difference of the boiling point is increased, thereby increasing the CS₂The recovery rate can also be improved₂And recovering the purity.

Description

Reclaim CS in the insoluble sulfur production process 2Method

Technical field

The present invention relates to distillation recovery CS in a kind of insoluble sulfur production process ₂Method.

Background technology

The chemical name of insoluble sulfur is the homopolymer of sulphur, is called for short IS, and it is a kind of vulcanizer of excellence, mainly is used as the vulcanizing agent of radial.In the insoluble sulfur production process, common sulphur aggregates into the transformation efficiency of insoluble sulfur more than 60%, obtain high-content IS, generally all adopts CS both at home and abroad ₂Make solvent, the soluble sulfur among the IS-60 (IS-60 is the polymerised sulphur that contains 40% left and right sides soluble sulfur) is dissolved in CS through extraction ₂In.And IS is insoluble to CS ₂, be suspended in CS ₂In, obtain the IS-95 powder by separation, and contain the CS of 40% left and right sides soluble sulfur of having an appointment ₂Mother liquor will reclaim CS by distillation ₂, recycle, must be not contain CS simultaneously ₂Soluble sulfur be separated at the bottom of the still kettle and recycle again.Traditional CS ₂Recovery method is to adopt the distillation of chuck still kettle, because the thermal conductivity of sulphur is very little, so heat-transfer effect is poor, at CS ₂In the still-process, the soluble sulfur concentration in the mother liquor increases and constantly separates out, distillation CS ₂The Shi Daliang heat absorption makes the suitable thickness of the sulphur of separating out, and last sulphur at the bottom of still contains the CS that has an appointment more than 20% ₂Very difficult quilt steams, and sulphur such at the bottom of the still is emitted can cause serious security incident and environmental pollution, simultaneously CS ₂Consume highly again, this is the ubiquitous problem of I S manufacturing firm, is also all making great efforts the best recovery technology of research and development.

Summary of the invention

The objective of the invention is to overcome the weak point in the existing production technique, provide a kind of and can avoid security incident and environmental pollution, effectively improve CS ₂Reclaim CS in the insoluble sulfur production process of the rate of recovery ₂Method.

Technical scheme of the present invention is: the concrete operation method of this recovery method is as follows: (1) adds earlier 1.8～2.2tCS in still kettle ₂Mother liquor is opened Helical Tube on Steam Generator steam valve in the still, and the still internal pressure is controlled at 0.14～0.16MPa, and after gas phase temperature reached 46～50 ℃, the flow with 1.4～1.6t/h added CS in still again ₂Mother liquor adds 28～32tCS in the order of classes or grades at school production altogether ₂Mother liquor;

(2) treat CS ₂Mother liquor is reinforced to be finished, and gas phase temperature rises to more than 50 ℃, opens major spiral pipe steam valve in the still, control pressure 0.4～0.5MPa, heating 100～140min;

(3) treat that temperature in the kettle reaches 130～140 ℃, straight pipe steam valve at the bottom of the unlatching still interpolation, vapor pressure 0.3～0.5MPa opens steam 14～18min, and when the cat head gas phase temperature rose to 90～95 ℃, distillation finished.

In above still-process, reclaim CS by condenser by the recovered overhead pipe ₂, open still after distillation finishes at the bottom of baiting valve emit Molten sulphur.

The present invention has adopted pressure-fired, water vapor extraction component distillation to reclaim CS ₂Novel process, pressure-fired distillation raising CS ₂Boiling point makes condenser refrigerant temperature and CS ₂The boiling point temperature difference strengthens, thereby has improved CS ₂Recovering effect, and strict control pressure-fired can prevent the discharge phenomenon in the still-process, raising recovery CS ₂Purity, guarantee to recycle CS ₂Quality.

Water vapor extraction azeotropic distillation technology is to utilize CS ₂Be slightly soluble in the characteristic of water, straight-through steam fed full-bodied at the bottom of the still kettle contain about 20% the CS of having an appointment ₂Molten sulphur in, with this part extremely difficult CS that reclaims ₂By extraction, component distillation is reclaimed, and under the reasonable cooperation of each processing condition and processing parameter, makes CS ₂The rate of recovery can reach more than 99%, noresidue CS almost in the recovery sulphur ₂, such sulphur is not emitted at the bottom of by still can cause security incident and environmental pollution.

Embodiment

Further specify the present invention below by embodiment.

With CS ₂Mother liquor is from CS ₂Mother liquor tank is pressed into CS with hydraulic pressure ₂Metering in the mother liquor test tank is then with 2 tons of CS ₂Mother liquor adds in the still kettle with canned-motor pump, open Helical Tube on Steam Generator steam valve in the still, and the steam regulation valve, the still internal pressure is controlled at positive 40mmHg (the differential manometer reading is equivalent to 0.153MPa), the cat head gas phase temperature is 46.5 ℃, and normal back adds CS with 1.5 tons flow feed rate per hour to still kettle ₂Mother liquor is treated the reinforced end of 30 tons of left and right sides mother liquors, and when gas phase temperature rose to 52 ℃, the differential manometer reading was 0～5mmHg and observes the no a large amount of CS in sulphur surface in the still from the still kettle visor ₂When bubble steams, open major spiral pipe steam valve in the still, during unlatching Helical Tube on Steam Generator steam valve in the still is left greatly, vapor pressure is controlled at 0.5MPa, heated 2 hours, make the interior complete melting of sulphur of still become liquid, liquidus temperature is 135 ℃ in the still, straight pipe cap relief valve at the bottom of the unlatching still interpolation, vapor pressure 0.4MPa, blow Molten sulphur rotation and rotation in the still, opened straight-through steam 15 minutes, the cat head gas phase temperature rises to 90 ℃ of distillations by 44 ℃ to be finished.In the above still-process, reclaim CS by condenser by the recovered overhead pipe ₂, after distillation finishes, open baiting valve at the bottom of the still, Molten sulphur in the still is pressed in the outdoor groove.

Claims (1)

1. reclaim CS in an insoluble sulfur production process ₂Method, the CS that suction filtration in producing is come out ₂Mother liquor quantitatively adds still kettle, utilizes the steam heating distillation, separates mother liquor, reclaims CS ₂, it is characterized in that concrete operation method is as follows:

(1) in still kettle, adds earlier 1.8～2.2tCS ₂Mother liquor is opened Helical Tube on Steam Generator steam valve in the still, and the still internal pressure is controlled at 0.14～0.16MPa, and after gas phase temperature reached 46～50 ℃, the flow with 1.4～1.6t/h added CS in still again ₂Mother liquor adds 28～32tCS altogether ₂Mother liquor;

(2) treat CS ₂Mother liquor is reinforced to be finished, and gas phase temperature rises to more than 50 ℃, opens major spiral pipe steam valve in the still, control pressure 0.4～0.5MPa, heating 100～140min;

(3) treat that temperature in the kettle reaches 130～140 ℃, straight pipe steam valve at the bottom of the unlatching still interpolation, vapor pressure 0.3～0.5MPa opens steam 14～18min, and when the cat head gas phase temperature rose to 90～95 ℃, distillation finished,

In above still-process, reclaim CS by condenser by the recovered overhead pipe ₂, open still after distillation finishes at the bottom of baiting valve emit Molten sulphur.