CN1060505C

CN1060505C - Producing process of solid chloroparaffin

Info

Publication number: CN1060505C
Application number: CN94109261A
Authority: CN
Inventors: 韩秋娴; 徐彦龙
Original assignee: Individual
Current assignee: Individual
Priority date: 1994-08-17
Filing date: 1994-08-17
Publication date: 2001-01-10
Anticipated expiration: 2014-08-17
Also published as: CN1122359A

Abstract

The present invention relates to the manufacturing technique of solid chloroparaffin, which belongs to the acyclic saturated compounds containing halogen atoms in organic chemistry. The present invention can greatly reduce harmful ingredients of tail gas discharged in the process of production so as to reduce environmental pollution, simplifies tail gas treatment, reduces the consumption of chlorine gas and reduces production cost. The present invention comprises the following procedures: heating paraffin in a storage tank, using CCl4 as solvents, carrying out chlorination in a reactor so as to reach 70% of chlorinity, putting the solvents to a middle tank from the storage tank to a middle tank, and carrying out washing and steam stripping so as to obtain solid products; in addition, separating and reclaiming washing water and the CCl4 for reuse, and processing tail gas of a chlorination reaction so as to obtain byproducts. The present invention is characterized in that the CCl4 is used as the solvents so as to carry out a third-stage intermittent chlorination reaction in the reactor with fusing paraffin.

Description

Producing process of solid chloroparaffin

The invention belongs to organic chemistry filed, contain the acyclic saturated compound of halogen atom, specifically a kind of chlorinity is the production technique of 70% solid chloroparaffin.

Traditional producing process of solid chloroparaffin is divided into two kinds of suspension method and solvent methods.But the weak point that suspension method exists is to eliminate moisture being difficult to of product, and solvability and thermostability are inferior than solvent method.

Solvent method carries out secondary usually and is interrupted chlorination reaction, with the paraffin that dissolves at 95～105 ℃ of following prechlorinations to chlorinity about 40%. add the CCl of 0.5～6 times of amount again ₄Solvent, the pressure normal pressure is to 6kgf/cm ², 70～120 ℃ of temperature, 12～30 hours reaction times.Chloride material is washed to pH6.5～7 and uses in the alkali again and pH7～7.5, can be refining by open steam.The CCl that stripping comes out ₄After the condensation separation drying for recycling, the material behind the desolventizing through cooling, grind, dry, sieve and finally obtain finished product.

" chlorine industry " 1987.9P22 page or leaf " evolution of clorafin and progress " literary composition has described the big auspicious company of U.S. solid chloroparaffin technological process in greater detail.Paraffin is stored in before chlorination in the heating storage tank, is interrupted chlorination reaction in being interrupted reactor, and chlorination reaches 70% to chlorinity, is moved to that medial launder washs and stripping, obtains solid phase prod, wash water, CCl ₄Separation and Recovery is used, and solid phase prod is pulverized and reached the designated size packing.The hydrogen chloride gas that unreacted chlorine and chlorination reaction produce neutralizes with white liquor after the absorption tower water absorbs again.

The weak point that above technology exists is to contain a large amount of unreacted chlorine and hydrogenchloride obnoxious flavour in the tail gas of discharging, and contaminate environment need be carried out twice vent gas treatment.The chlorine consumption is higher in process of production, is more than 1840 kilograms/ton.

The objective of the invention is to improve chlorinity and be 70% producing process of solid chloroparaffin, make and discharge the contained obnoxious flavour amount of tail gas and reduce greatly, reduce environmental pollution, simplify vent gas treatment, and reduce chlorine consumption in process of production, can reduce production costs like this.

The present invention is achieved in that and earlier paraffin is heated in storage tank, with CCl ₄Do solvent chlorination in reactor and reach 70%, be moved to that medial launder washs, neutralization and stripping obtain solid phase prod, through super-dry, pulverize and reach the designated size packing, again with wash water, CCl to chlorinity ₄Separation and Recovery is used, the treated byproduct hydrochloric acid that obtains of chlorination reaction tail gas, and feature of the present invention is: CCl ₄Make solvent and dissolve paraffin in reactor, to carry out three grades of interruption chlorination reactions, promptly the melt paraffin after the heating enters reactor No. 1, liquid material enters No. 2 reactors by No. 1 reactor and reenters reactor No. 3, chlorine then enters No. 2 reactors by No. 3 reactors and enters reactor again No. 1, carries out countercurrent reaction.Three grades of conditions of being interrupted chlorination reaction are; 40～90 ℃ of temperature of reaction, the reaction times is 20～60 hours, when chlorine is entered No. 2 reactors and is entered No. 1 reactor again by No. 3 reactor its absolute pressure in 0～0.1MPa scope step by step from large to small.Three grades are interrupted reacted tail gas and absorb through the absorption tower water and become hydrochloric acid, absorb the tail gas emptying behind the hydrochloric acid, and chloride and hydrogenchloride amount is below 10ppm.

CCl ₄Make solvent, add heated paraffin and carry out three grades when being interrupted reaction in reactor, it is better to be controlled at following conditioned response: 45～70 ℃ of temperature of reaction, reaction pressure 0～0.1MPa, 25～50 hours reaction times.

CCl ₄Make solvent, add heated paraffin and in reactor, carry out three grades when being interrupted reaction, be controlled at following conditioned response the best: 47～56 ℃ of temperature of reaction, reaction pressure 0～0.05MPa, 31～35 hours reaction times.

The present invention compares with traditional producing process of solid chloroparaffin, has following useful effect;

The present invention is owing to adopted three grades of chlorination process, Cl ₂Chlorine obtains complete reaction when reacting with paraffin in reactor, makes to discharge that chlorinity and hydrogen chloride gas reduce greatly in the tail gas, and the chloride and hydrogenchloride amount of the tail gas of being discharged has been improved production environment below 10ppm, reduced environmental pollution effectively.

2, because discharge tail gas is chloride and the hydrogenchloride amount reduces greatly, the present invention only needs tail gas is carried out disposable processing, tail gas water in the absorption tower is absorbed as hydrochloric acid, and background technology needs tail gas is done twice processing, except that water is absorbed as hydrochloric acid, also need to neutralize with caustic soda again.The tail gas primary treatment has been saved the raw material caustic soda than twice processing, has reduced use equipment and work-yard, has reduced production cost.

3, the present invention makes the chlorine consumption reduce greatly in process of producing product.Adopting traditional technology chlorine consumption is more than 1840 kilograms/ton, adopts chlorine consumption of the present invention to drop to 1400～1500 kilograms/ton, has reduced production cost, and remarkable economic efficiency is arranged.

The present invention compares than background technology, reduces production costs 20%.

Be described further below in conjunction with embodiment:

Table 1 is three grades and is interrupted the processing condition that chlorination reaction adopts.Table 1:

Products material adopts 56 ℃ of refined white waxs that sell in market in listed each embodiment of table 1, and chlorine adopts liquid chlorine, and purity is more than 99%.Three grades of chlorination processes are intermittent operation, and the chlorination tank capacity is 0.5～3 meter ³, logical chlorine dose 5～20m ³/ h, temperature of reaction maintains 40～90 ℃, 1～3 day reaction time.Purification apparatus adopts 4～6 meters ³Corrosion protective lining equipment, by the air depickling, stripping 3～4 hours, temperature is controlled at 50～110 ℃, add again alkaline solution a little, obtain C ₂₄H ₂₉Cl ₂₁Product, carry out drying, pulverize, reach designated size packing.

Claims

1, a kind of producing process of solid chloroparaffin the steps include: earlier paraffin to be heated in storage tank, with CCl ₄Do solvent chlorination in reactor and reach 70%, be moved to that medial launder washs, neutralization and stripping obtain solid phase prod, through super-dry, pulverize and reach the designated size packing to chlorinity; In addition again with wash water, CCl ₄Separation and Recovery is used, and the treated byproduct that obtains of chlorination reaction tail gas is characterized in that: CCl ₄Make solvent and dissolve paraffin in reactor, to carry out three grades of interruption chlorination reactions, three grades of conditions of being interrupted chlorination reaction are: 40～90 ℃ of temperature of reaction, reaction times is 20～60 hours, cl gas flow is that to flowing to paraffin opposite countercurrent reaction, chlorine enter three reactor and reduce step by step in 0～0.1MPa scope to flowing out its reaction pressure.

2, producing process of solid chloroparaffin according to claim 1 is characterized in that chlorination reaction tail gas only need carry out primary treatment, promptly is absorbed as hydrochloric acid through the absorption tower water.

3, producing process of solid chloroparaffin according to claim 1 is characterized in that three grades of conditions of being interrupted chlorination reaction are 45～70 ℃ of temperature of reaction, reaction pressure 0～0.1MPa, 25～50 hours reaction times.

4, producing process of solid chloroparaffin according to claim 1 is characterized in that: three grades of conditions of being interrupted reaction are 47～56 ℃ of temperature of reaction, reaction pressure 0～0.5MPa, 31～35 hours reaction times.