CN103804319A

CN103804319A - Process for recycling accelerator M from residual liquid of rubber accelerator CZ distillation still

Info

Publication number: CN103804319A
Application number: CN201410079311.1A
Authority: CN
Inventors: 李明; 秦怀光; 杨小岗
Original assignee: WANTONG RUBBER ACCELERATOR CO Ltd
Current assignee: WANTONG RUBBER ACCELERATOR CO Ltd
Priority date: 2014-03-06
Filing date: 2014-03-06
Publication date: 2014-05-21

Abstract

The invention relates to a process for recycling an accelerator M from the residual liquid of a rubber accelerator CZ distillation still in the field of the fine chemical industry. The technical scheme is that the process comprises the following steps: (1) cooling the residual liquid in the rubber accelerator CZ distillation still by use of a cooling tower, then pumping the residual liquid into an oxidation reaction kettle by use of a chemical pump, metering the quantity of a mother solution pumped into the reaction kettle by use of a pipeline electromagnetic flow meter, and calculating the quantity of the used sulfuric acid in combination with the PH value of the residual liquid in the oxidation reaction kettle and the quantity of the added mother solution; (2) slowly dripping the metered sulfuric acid solution into the residual liquid of the kettle according to a rule that the solution is dripped slowly in the initial stage and the terminal stage and dripped rapidly in the middle stage, and controlling the PH value of the final solution to be within 4-5; (3) after the reaction is ended, putting the materials in a vacuum filtration tank for a filtration process and then obtaining a material accelerator M. The process has the beneficial effects that the process can be used for recycling the accelerator M discharged from the residual liquid of the kettle, thus the consumption per ton is reduced, the yield is increased, and the pressure on sewage treatment is relieved as well.

Description

Rubber accelerator CZ still kettle raffinate reclaims captax technique

Technical field

The rubber accelerator CZ still kettle raffinate the present invention relates in field of fine chemical reclaims captax technique.

Background technology

Rubber accelerator CZ is a kind of conventional thiofide, the sulfenamide that exceeds the speed limit in genus, and chemical name is N-cyclohexyl-2-[4-morpholinodithio sulphenamide, it is the delayed action accelerator that a kind of height is active, scorching quality is good, process safety, and curing time is short, be applicable to various rubber, variable color is slight, no blooming, and cross-linked rubber is ageing-resistant, tensile strength, surely to stretch ability all better, mainly for the manufacture of industrial rubber articles such as tire, sebific duct, rubber overshoes, electric wires; Current rubber industry and vulcanization accelerator industry are all subject to the puzzlement of carinogenicity nitrosamine, NOBS and other secondary amine structural promotors can produce the nitrosamine that has carinogenicity between curing time, non-carcinogenesis problem of the sulfenamide vulcanization accelerator of the primary amine structures such as accelerant CZ, thereby be subject to generally attention and the research and development of industry.

In existing technique, captax drops in hexahydroaniline solution, captax reacts rapidly agglomerate with hexahydroaniline, generate larger, harder blocks of solid, this blocks of solid appearance is reaction promoter for generation M amine salt, inside is unreacted captax, though this process has agitator to stir and the grinding of grinding pump, but the two reacts agglomerate and generates blocks of solid and this chemical property of particle due to captax and hexahydroaniline, finally cause the promotor captax of some not carry out fully contact and react, this procedure being oxidized with NaClO on the one hand, pH value generally maintains 12.0 left and right, that is to say that solution presents alkalescence, be C(OH ^-) > C(H ⁺), this process is understood some and is not participated in the captax of reaction, salify in alkaline environment (captax-Na salt), the rubber accelerator CZ material that part reaction generates in reaction process on the other hand, be dissolved in hexahydroaniline solution, in centrifuge washing process subsequently, can enter in mother liquor with washings, and then through still kettle, but this part captax-Na salt, be dissolved in the rubber accelerator CZ in hexahydroaniline solution, in still-process, can not separate out also and can not be distilled out of, entering trench with still kettle raffinate enters between water treatment vehicle, in this part still kettle raffinate, contain ester class, salt, captax-Na that a part is dissolved, the mixture of rubber accelerator CZ and other impurity etc. that hexahydroaniline solution dissolves, a kind of organic waste water and brine waste of high density, directly discharge not only can cause between water treatment vehicle COD index higher, and the rubber accelerator CZ material of a part of captax-Na and hexahydroaniline dissolving, also caused the loss of material with the discharge of still liquid.

Summary of the invention

The problem existing for prior art, technician finds that in long-term R&D and production process the rubber accelerator CZ still kettle raffinate of a kind of energy recycling reclaims captax technique.

Technical scheme: described processing step is:

(1), the interior raffinate of rubber accelerator CZ still kettle is after cooling tower cooling, squeeze in oxidizing reactor with chemical pump, the amount of squeezing into mother liquor in reactor with the metering of pipe electromagnetic under meter, in conjunction with the numerical value of raffinate PH in oxidizing reactor and the add-on of mother liquor, calculates the consumption of sulfuric acid; (2), slow the sulphuric acid soln measuring stream is added in still raffinate, drips and adopt slow, the middle fast principle in two, the pH value of terminal solution is controlled between 4-5;

(3), reacted after, material is put into vacuum suction filtration tank and is carried out filtration treatment, collects material captax.

Beneficial effect: this technology can be by the captax recycling of discharging in still raffinate, not only can reduce ton consumption, improves yield, also helps the pressure that alleviates sewage disposal, and expection can produce good economic benefit and social benefit.

Accompanying drawing explanation: nothing.

Embodiment

Embodiment: the present embodiment main technological steps is:

(1) the mother liquor terminal in still kettle record tail heat up in a steamer amine below 1.2% after, sample examination COD of sewage, open still kettle bottom valve, put into pond, open chemical pump and be down to 40 ℃ through cooling tower, then cooling good still raffinate is squeezed in oxidizing reactor, recorded numerical value 3.8 M3 of magnetic flow meter, record the pH value of still raffinate;

(2) open reactor and stir, add sulfuric acid, until pH value of solution=5.0～6.0;

(3) after being added dropwise to complete, continue to stir 30Min, until there is more loose material to generate in solution, solution colour is limpid, then puts into suction filtration tank and open vacuum pump suction filtration gained captax, recycles in CZ oxidation operation;

This batch of this analysis report:

Claims

1. rubber accelerator CZ still kettle raffinate reclaims captax technique: it is characterized in that: described processing step is:

(1), the interior raffinate of rubber accelerator CZ still kettle is after cooling tower cooling, squeeze in oxidizing reactor with chemical pump, the amount of squeezing into mother liquor in reactor with the metering of pipe electromagnetic under meter, in conjunction with the numerical value of raffinate PH in oxidizing reactor and the add-on of mother liquor, calculates the consumption of sulfuric acid; (2), slow the sulphuric acid soln measuring stream is added in still raffinate, drips and adopt slow, the middle fast principle in two, the pH value of terminal solution is controlled between 4-5; (3), reacted after, material is put into vacuum suction filtration tank and is carried out filtration treatment, collects material captax.