CN103204479A - Production method for high-content insoluble sulfur - Google Patents

Abstract

The invention discloses a production method for high-content insoluble sulfur. The production method includes heating common sulfur to be melted, and controlling the temperature at 130-145 DEG C, adding attapulgite powder and nano-silica both with weights amounting for 1-2% of sulfur weight, stirring evenly, pushing the melt into a temperature raising tank by a sulfur metering pump, raising the temperature automatically and controlling the temperature at 370-450 DEG C, atomizing, quenching, solidifying and coating the melt and the like. By the production method, product yield, high-thermal stability and dispersibility are greatly improved, and finished products can fully meet the requirements of radial tires on insoluble sulfur with high content, high thermal stability and high dispersibility.

Description

A kind of production method of high content insoluble sulfur

Technical field

The present invention relates to a kind of Manufacture of insoluble sulphur method, relate in particular to a kind of production method of high content insoluble sulfur.

Background technology

Insoluble sulfur is a kind of allotropic substance of common sulphur, it is the linear polymeric that is polymerized by a large amount of sulphur atoms, be insoluble to dithiocarbonic anhydride, also be insoluble to rubber, so be referred to as insoluble sulfur or polymerization sulphur, formal name used at school is high molecular polymerization sulphur (English name is INSOLUBIESULFUR, is called for short IS), and it is widely used in the manufacturing of rubber items such as tire mainly as a kind of vulcanizing agent of rubber industry.Existing insoluble sulfur is dispersed bad in Rubber processing, causes the rubber vulcanization heterogeneity easily, influences the processing characteristics of sizing material, thereby influences the performance of rubber item.

Summary of the invention

The present invention provides a kind of production method of high content insoluble sulfur in order to remedy the deficiencies in the prior art, and by present method, product yield, high thermal stability and dispersiveness all have significantly raising.

The present invention is achieved by the following technical solutions.

A kind of production method of high content insoluble sulfur is characterized in that comprising the steps:

(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 130-145 ℃; Add and to be equivalent to the attapulgite powder of sulphur weight 1-2% and the nano silicon of 1-2%, stir, melt is squeezed in the jar that heats up with the sulphur volume pump, heat up automatically and control temperature at 370 ℃-450 ℃;

(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur liquid uniform atomizing of atomizing nozzle with fusion, in the quenching synthesizer, fully contact with 30-35 ℃ quenching liquid from all directions then, quick cooling forms uniform insoluble sulfur particle and is suspended in the quenching liquid; Wherein, quenching liquid is dithiocarbonic anhydride;

(3) solidify, extract, separate: mixed suspension enters in the reactor that has whipping appts, and insoluble sulfur is cured in device, and solidification value is 40-60 ℃, and be 1-2h set time; Material repeatedly washed extraction through dithiocarbonic anhydride after curing was finished in reactor, and filter residue obtains insolubility sulphur;

(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%-1.0%, under 3000-4000 rev/min, stirred 10-15 minute, coat, described stablizer is mixed by the raw material of following weight part: catechol 1-2, ether 10-12, ferrocene 1-2, anti-aging agent OD 1-2, nano-attapulgite powder 0.1-0.2, urotropine 0.1-0.2;

(5) drying: negative pressure drying obtains fineness 100-200 purpose insoluble sulfur powder;

(6) screening, oil-filled: the insoluble sulfur powder is through screening, be distributed into finished product after oil-filled.

Production method of the present invention, product yield, high thermal stability and dispersiveness all have significantly raising, and products obtained therefrom can satisfy radial fully to the requirement of " three height " insoluble sulfur.

Embodiment

A kind of production method of high content insoluble sulfur comprises the steps:

(1) molten sulphur, intensification: sulphur is melted in the common sulphur heating of 500 grams, and the control temperature is 140-145 ℃; Add and to be equivalent to the attapulgite powder of sulphur weight 1% and 1% nano silicon, stir, melt is squeezed in the jar that heats up with the sulphur volume pump, heat up automatically and control temperature at 420 ℃-450 ℃;

(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur liquid uniform atomizing of atomizing nozzle with fusion, in the quenching synthesizer, fully contact with 32-35 ℃ quenching liquid from all directions then, quick cooling forms uniform insoluble sulfur particle and is suspended in the quenching liquid; Wherein, quenching liquid is dithiocarbonic anhydride;

(3) solidify, extract, separate: mixed suspension enters in the reactor that has whipping appts, and insoluble sulfur is cured in device, and solidification value is 40-60 ℃, and be 1-2h set time; Material repeatedly washed extraction through dithiocarbonic anhydride after curing was finished in reactor, and filter residue obtains insolubility sulphur 231 grams;

(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 1.0%, under 3000-4000 rev/min, stirred 10-15 minute, coat, described stablizer is mixed by the raw material of following weight part (gram): catechol 2, ether 12, ferrocene 2, anti-aging agent OD 2, nano-attapulgite powder 0.1, urotropine 0.1;

(5) drying: negative pressure drying obtains fineness 100-200 purpose insoluble sulfur powder;

(6) screening, oil-filled: the insoluble sulfur powder is through screening, be distributed into finished product after oil-filled.

After testing, finished product insoluble sulfur content is that the high thermal stability of 95.6%, 105 ℃/15min is that the high thermal stability of 82%, 120 ℃/15min is 53%.

Claims (1)

1. the production method of a high content insoluble sulfur is characterized in that comprising the steps:

(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 130-145 ℃; Add and to be equivalent to the attapulgite powder of sulphur weight 1-2% and the nano silicon of 1-2%, stir, melt is squeezed in the jar that heats up with the sulphur volume pump, heat up automatically and control temperature at 370 ℃-450 ℃;

(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur liquid uniform atomizing of atomizing nozzle with fusion, in the quenching synthesizer, fully contact with 30-35 ℃ quenching liquid from all directions then, quick cooling forms uniform insoluble sulfur particle and is suspended in the quenching liquid; Wherein, quenching liquid is dithiocarbonic anhydride;

(3) solidify, extract, separate: mixed suspension enters in the reactor that has whipping appts, and insoluble sulfur is cured in device, and solidification value is 40-60 ℃, and be 1-2h set time; Material repeatedly washed extraction through dithiocarbonic anhydride after curing was finished in reactor, and filter residue obtains insolubility sulphur;

(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%-1.0%, under 3000-4000 rev/min, stirred 10-15 minute, coat, described stablizer is mixed by the raw material of following weight part: catechol 1-2, ether 10-12, ferrocene 1-2, anti-aging agent OD 1-2, nano-attapulgite powder 0.1-0.2, urotropine 0.1-0.2;

(5) drying: negative pressure drying obtains fineness 100-200 purpose insoluble sulfur powder;

(6) screening, oil-filled: the insoluble sulfur powder is through screening, be distributed into finished product after oil-filled.