CN104692336A - High-quality cold-resistant insoluble sulfur and preparation method thereof - Google Patents
High-quality cold-resistant insoluble sulfur and preparation method thereof Download PDFInfo
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- CN104692336A CN104692336A CN201510071557.9A CN201510071557A CN104692336A CN 104692336 A CN104692336 A CN 104692336A CN 201510071557 A CN201510071557 A CN 201510071557A CN 104692336 A CN104692336 A CN 104692336A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/12—Insoluble sulfur (mu-sulfur)
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Abstract
The invention discloses high-quality cold-resistant insoluble sulfur. The high-quality cold-resistant insoluble sulfur is characterized by being prepared from the following raw materials in parts by weight: 100 parts of sulphur powder, 0.8-2.3 parts of white carbon black, 1-2 parts of aluminum nitride powder, 2-3 parts of emery powder, 0.6-0.9 part of octadecanamide, 3-5 parts of nano silicon power, 0.1-0.3 part of olive oil, 0.05-0.09 part of ABS high glue powder, 0.2-0.4 part of potassium bromide, 0.3-0.6 part of graphene, 0.03-0.06 part of an anti-aging agent 4030, 5-8 parts of acetyl tributyl citrate and a proper amount of water. Modified white carbon black is added in the preparation process by a low-temperature liquid phase method as an anti-static agent, so that the static electricity of the product can be removed; and the content of insoluble sulfur is improved; meanwhile, 0.1% of pentaerythritol aqueous solution is selected as a quenching liquid, so that the high-quality cold-resistant insoluble sulfur has the characteristics of low cost, significant quenching effect, and high extraction efficiency; an organic solvent can be recycled and repeatedly utilized; and the cold-resistant property of a rubber product can be improved by adding the acetyl tributyl citrate. Through the method, the yield, the high thermal stability and the dispersity of the product are greatly improved; cycle use of raw materials is realized; the production cost is reduced; and the preparation method belongs to the environmental protection technology.
Description
Technical field
The present invention relates to insoluble sulfur preparing technical field, be specifically related to cold-resistant type insoluble sulfur of a kind of high-quality 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 cold-resistant type insoluble sulfur of a kind of high-quality and preparation method thereof, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this:
The cold-resistant type insoluble sulfur of a kind of high-quality, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.8-2.3, aluminum nitride powder 1-2, lapis amiridis 2-3, stearic amide 0.6-0.9, nano silica fume 3-5, sweet oil 0.1-0.3, ABS high glue powder 0.05-0.09, Potassium Bromide 0.2-0.4, Graphene 0.3-0.6, anti-aging agent 4030 0.03-0.06, tributyl acetylcitrate 5-8, suitable quantity of water.
The preparation method of the cold-resistant type insoluble sulfur of described a kind of high-quality, is characterized in that comprising the following steps:
(1) white carbon black, aluminum nitride powder, ABS high glue powder, Graphene 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, tributyl acetylcitrate stirs, continue to be warming up to 220-310 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 lapis amiridis, Potassium Bromide, nano silica fume, sweet oil 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, there is cost low, quenching Be very effective, extraction efficiency is high, the feature of the recyclable recycling of organic solvent, add the cold performance that tributyl acetylcitrate can improve rubber product, pass through present method, product yield, high thermal stability and dispersiveness all have and significantly improve, and achieve recycling of raw material, reduce production cost, belong to environmental protection technique.
Embodiment
The cold-resistant type insoluble sulfur of described a kind of high-quality, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 1.8, aluminum nitride powder 1, lapis amiridis 3, stearic amide 0.7, nano silica fume 3, sweet oil 0.1, ABS high glue powder 0.06, Potassium Bromide 0.2, Graphene 0.4, anti-aging agent 4,030 0.05, tributyl acetylcitrate 8, suitable quantity of water.
Making method comprises the following steps:
(1) white carbon black, aluminum nitride powder, ABS high glue powder, Graphene 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, tributyl acetylcitrate stirs, continue to be warming up to 220-310 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 lapis amiridis, Potassium Bromide, nano silica fume, sweet oil 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 86.1%;
The high thermal stability of (2) 105 DEG C/15min is the high thermal stability of 85.9%, 120 DEG C/15min is 51.5%.
Claims (3)
1. the cold-resistant type insoluble sulfur of high-quality, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.8-2.3, aluminum nitride powder 1-2, lapis amiridis 2-3, stearic amide 0.6-0.9, nano silica fume 3-5, sweet oil 0.1-0.3, ABS high glue powder 0.05-0.09, Potassium Bromide 0.2-0.4, Graphene 0.3-0.6, anti-aging agent 4030 0.03-0.06, tributyl acetylcitrate 5-8, suitable quantity of water.
2. the making method of the cold-resistant type insoluble sulfur of a kind of high-quality according to claim 1, is characterized in that comprising the following steps:
(1) white carbon black, aluminum nitride powder, ABS high glue powder, Graphene 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, tributyl acetylcitrate stirs, continue to be warming up to 220-310 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 lapis amiridis, Potassium Bromide, nano silica fume, sweet oil 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 the cold-resistant type insoluble sulfur of a kind of high-quality according to claim 2, is characterized in that described quenching liquid is the 0.1% tetramethylolmethane aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510071557.9A CN104692336A (en) | 2015-02-11 | 2015-02-11 | High-quality cold-resistant insoluble sulfur and preparation method thereof |
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| CN201510071557.9A CN104692336A (en) | 2015-02-11 | 2015-02-11 | High-quality cold-resistant insoluble sulfur and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730648A (en) * | 2012-07-03 | 2012-10-17 | 山东尚舜化工有限公司 | Production method of high-quality insoluble sulfur |
| CN103303873A (en) * | 2013-05-23 | 2013-09-18 | 上海京海（安徽）化工有限公司 | Preparation method of modified high-dispersion high-thermal-stability insoluble sulfur |
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- 2015-02-11 CN CN201510071557.9A patent/CN104692336A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730648A (en) * | 2012-07-03 | 2012-10-17 | 山东尚舜化工有限公司 | Production method of high-quality insoluble sulfur |
| CN103303873A (en) * | 2013-05-23 | 2013-09-18 | 上海京海（安徽）化工有限公司 | Preparation method of modified high-dispersion high-thermal-stability insoluble sulfur |
Non-Patent Citations (1)
| Title |
|---|
| 李双文: ""不溶性硫磺的研究和开发进展"", 《精细化工原料及中间体》 * |
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Application publication date: 20150610 |