CN104692334A - Insoluble sulfur with high dispersibility and high fineness and preparation method of insoluble sulfur - Google Patents

Abstract

The invention discloses insoluble sulfur with high dispersibility and high fineness. The insoluble sulfur is characterized by being prepared from the following raw materials in parts by weight: 100 parts of sulfur powder, 0.6-0.9 part of white carbon black, 0.4-0.7 part of cobaltous oxide, 0.04-0.08 part of a silane coupling agent KH590, 0.7-1.5 parts of benzoic acid, 0.05-0.09 part of hexamethylenetetramine, 0.1-0.3 part of zinc acetate, 0.2-0.4 part of calcium molybdate, 2-3 parts of vaseline, 1-2 parts of nanometer rice hull ashes, 7-9 parts of nanometer silicon carbide, 1.2-3.2 parts of butyl oleate and a proper amount of water. Modified white carbon black is added as an antistatic agent in the preparation process by a low-temperature liquid phase method; static electricity of the product can be removed; the content of the insoluble sulfur is improved; and meanwhile, 0.1% pentaerythritol water solution is selected as quenching liquid, so that the cost is low; the effect is significant; the prepared insoluble sulfur has the characteristics of high heat stability, high dispersibility and high fineness; and the technological operation is simple, high in efficiency, high in safety, and suitable for industrial production.

Description

A kind of polymolecularity high fineness insoluble sulfur and preparation method thereof

Technical field

The present invention relates to insoluble sulfur preparing technical field, be specifically related to a kind of polymolecularity high fineness insoluble sulfur and preparation method thereof.

Background technology

Insoluble sulfur is also called plastic sulfur or polymerised sulphur, by the linear polymeric of a large amount of sulphur atom by being polymerized, relative molecular mass can reach tens thousand of, it is a kind of nontoxic, flammable yellow powder, gain the name because it is insoluble to dithiocarbonic anhydride, it is the allotropic substance of the high polymeric species of common sulphur and macromolecule modified kind.Insoluble sulfur is a kind of efficient vulcanizer, and have distributional stability in sizing material good, goods vulcanization crosslinking point evenly can overcome sizing material surface " bloom ", promotes the advantages such as the bonding of rubber and steel wire or chemical fibre cord thread.At present, the insoluble sulfur overwhelming majority is used for rubber industry, has become the dedicated vulcanization agent of producing high quality radial.

Low temperature liquid polymerization process prepares insoluble sulfur only by sulphur melt overheat, sulphur is not needed to gasify, temperature is relatively low, there is the advantage that energy consumption is low, working condition is relatively gentle, wherein the most key process procedure is chilling and solidification, both affect the performance of the finished product to a great extent, and the insoluble sulfur produced in prior art exists the defects such as dispersiveness is not good, thermostability is not high, it is low to sample, complex process.

Summary of the invention

Object of the present invention is just to provide a kind of polymolecularity high fineness insoluble sulfur and preparation method thereof, to overcome the deficiencies in the prior art.

The object of the present invention is achieved like this:

A kind of polymolecularity high fineness insoluble sulfur, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.6-0.9, cobalt oxide 0.4-0.7, silane coupling agent KH590 0.04-0.08, phenylformic acid 0.7-1.5, Wu Tuoluo product 0.05-0.09, zinc acetate 0.1-0.3, calcium molybdate 0.2-0.4, Vaseline 2-3, nanometer rice hull ash 1-2, nanometer silicon carbide 7-9, butyl oleate 1.2-3.2, suitable quantity of water.

The preparation method of described a kind of polymolecularity high fineness insoluble sulfur, is characterized in that comprising the following steps:

(1) white carbon black, zinc acetate, silane coupling agent KH590 are added suitable quantity of water and be heated to 50-60 DEG C of ultrasonic wave dispersion grinding 3-6 hour, spraying dry obtains modified white carbon black;

(2) SULPHUR POWDER is heated to molten state at 120-145 DEG C, is warming up to that 160 DEG C add modified white carbon black, Vaseline, cobalt oxide stir, continue to be warming up to 220-305 DEG C, insulation 1-2h;

(3) high temperature sulphur liquid obtained above is poured into rapidly in normal temperature quenching liquid cool rapidly, form uniform insoluble sulfur particle and be suspended in quenching liquid;

(4) suspension liquid obtained after quenching is placed in the reactor with whipping appts and is cured 4-4.5h at 50-60 DEG C, obtain the thick product of insoluble sulfur;

(5) thick for insoluble sulfur product is added nanometer rice hull ash, nanometer silicon carbide, butyl oleate and other remaining components high-speed stirring 10-15 minute, carry out coated, through negative pressure drying, grinding, screening, oil-filledly obtain insoluble sulfur powder.

The present invention has following beneficial effect: the present invention adopts low temperature liquid polymerization process in preparation process, to add modified white carbon black as static inhibitor, the electrostatic of product can be eliminated and improve the content of insoluble sulfur, it is quenching liquid that the present invention simultaneously chooses the 0.1% tetramethylolmethane aqueous solution, cost is low, Be very effective, the insoluble sulfur prepared has the characteristic of high thermal stability, polymolecularity, high fineness, and the simple efficiency of technological operation is high, security is high, is applicable to suitability for industrialized production.

Embodiment

Described a kind of polymolecularity high fineness insoluble sulfur, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.7, cobalt oxide 0.5, silane coupling agent KH590 0.06, phenylformic acid 0.9, Wu Tuoluo product 0.05, zinc acetate 0.1, calcium molybdate 0.2, Vaseline 2, nanometer rice hull ash 1, nanometer silicon carbide 8, butyl oleate 1.9, suitable quantity of water.

Making method comprises the following steps:

(1) white carbon black, zinc acetate, silane coupling agent KH590 are added suitable quantity of water and be heated to 50-60 DEG C of ultrasonic wave dispersion grinding 3-6 hour, spraying dry obtains modified white carbon black;

(2) SULPHUR POWDER is heated to molten state at 120-145 DEG C, is warming up to that 160 DEG C add modified white carbon black, Vaseline, cobalt oxide stir, continue to be warming up to 220-305 DEG C, insulation 1-2h;

(3) high temperature sulphur liquid obtained above is poured into rapidly in normal temperature quenching liquid cool rapidly, form uniform insoluble sulfur particle and be suspended in quenching liquid;

(4) suspension liquid obtained after quenching is placed in the reactor with whipping appts and is cured 4-4.5h at 50-60 DEG C, obtain the thick product of insoluble sulfur;

(5) thick for insoluble sulfur product is added nanometer rice hull ash, nanometer silicon carbide, butyl oleate and other remaining components high-speed stirring 10-15 minute, carry out coated, through negative pressure drying, grinding, screening, oil-filledly obtain insoluble sulfur powder.

The technical parameter index of the insoluble sulfur using the present invention to produce is as follows:

(1) finished product dispersity of insoluble sulfur is good, and content is 92.6%;

(2), through 105 DEG C, after 15 min heat treated, the thermally-stabilised rate of insoluble sulfur reaches 92.4%.

Claims (3)

1. a polymolecularity high fineness insoluble sulfur, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.6-0.9, cobalt oxide 0.4-0.7, silane coupling agent KH590 0.04-0.08, phenylformic acid 0.7-1.5, Wu Tuoluo product 0.05-0.09, zinc acetate 0.1-0.3, calcium molybdate 0.2-0.4, Vaseline 2-3, nanometer rice hull ash 1-2, nanometer silicon carbide 7-9, butyl oleate 1.2-3.2, suitable quantity of water.

2. the making method of a kind of polymolecularity high fineness insoluble sulfur according to claim 1, is characterized in that comprising the following steps:

(1) white carbon black, zinc acetate, silane coupling agent KH590 are added suitable quantity of water and be heated to 50-60 DEG C of ultrasonic wave dispersion grinding 3-6 hour, spraying dry obtains modified white carbon black;

(2) SULPHUR POWDER is heated to molten state at 120-145 DEG C, is warming up to that 160 DEG C add modified white carbon black, Vaseline, cobalt oxide stir, continue to be warming up to 220-305 DEG C, insulation 1-2h;

(3) high temperature sulphur liquid obtained above is poured into rapidly in normal temperature quenching liquid cool rapidly, form uniform insoluble sulfur particle and be suspended in quenching liquid;

(4) suspension liquid obtained after quenching is placed in the reactor with whipping appts and is cured 4-4.5h at 50-60 DEG C, obtain the thick product of insoluble sulfur;

(5) thick for insoluble sulfur product is added nanometer rice hull ash, nanometer silicon carbide, butyl oleate and other remaining components high-speed stirring 10-15 minute, carry out coated, through negative pressure drying, grinding, screening, oil-filledly obtain insoluble sulfur powder.

3. the making method of a kind of polymolecularity high fineness insoluble sulfur according to claim 2, is characterized in that described quenching liquid is the 0.1% tetramethylolmethane aqueous solution.