CN104671215A - Weather-proof anti-aging high-thermal-stability insoluble sulfur and production method thereof - Google Patents
Weather-proof anti-aging high-thermal-stability insoluble sulfur and production method thereof Download PDFInfo
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- CN104671215A CN104671215A CN201510071511.7A CN201510071511A CN104671215A CN 104671215 A CN104671215 A CN 104671215A CN 201510071511 A CN201510071511 A CN 201510071511A CN 104671215 A CN104671215 A CN 104671215A
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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 weather-proof anti-aging high-thermal-stability insoluble sulfur, which is characterized by being prepared from the following raw materials in parts by weight: 100 parts of sulfur powder, 0.5-1.2 parts of white carbon black, 0.2-0.4 part of urea, 0.1-0.3 part of magnesium carbonate, 4-7 parts of attapulgite, 1-2 parts of nanotitanium dioxide, 0.03-0.07 part of accelerant CZ, 2-3 parts of dioctyl phthalate, 6-9 parts of hexachlorocyclopentadiene, 2-4 parts of p-tolyl isocyanate, 0.3-0.5 part of anti-aging agent 2246, and a proper amount of water. According to the method, the energy consumption is low, and static electricity of the product can be eliminated and the content of insoluble sulfur can be increased by adding modified white carbon black serving as an antistatic agent during preparation through a low-temperature liquid method; by taking 0.1% of pentaerythritol water solution as a cold quenching liquid, the cost is low, and the effect is obvious; and by adding nanotitanium dioxide, the weather-proof property of rubber finished products can be enhanced and the dispersity of insoluble sulfur can be improved; and according to the prepared insoluble sulfur, the conversion rate is high, the heat resistance and natural degradation capabilities are also good.
Description
Technical field
The present invention relates to insoluble sulfur preparing technical field, be specifically related to a kind of weather-proof anti-aging high-thermostability 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 weather-proof anti-aging high-thermostability 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 weather-proof anti-aging high-thermostability insoluble sulfur, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.5-1.2, urea 0.2-0.4, magnesiumcarbonate 0.1-0.3, attapulgite 4-7, nano titanium oxide 1-2, accelerant CZ 0.03-0.07, dioctyl phthalate (DOP) 2-3, hexachlorocyclopentadiene 6-9, to toluene diisocyanate 2-4, antioxidant 2246 0.3-0.5, suitable quantity of water.
The preparation method of described a kind of weather-proof anti-aging high-thermostability insoluble sulfur, is characterized in that comprising the following steps:
(1) white carbon black, urea, accelerant CZ 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, nano titanium oxide 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 attapulgite, dioctyl phthalate (DOP), hexachlorocyclopentadiene 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: method energy consumption of the present invention is lower, low temperature liquid polymerization process is adopted 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, add nano titanium oxide can improve the weathering resistance of rubber product and the dispersiveness of insoluble sulfur, the transformation efficiency of the insoluble sulfur utilizing the present invention to obtain is higher, thermotolerance and against natural degeneration ability also better.
Embodiment
The weather-proof anti-aging high-thermostability insoluble sulfur of described one, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.8, urea 0.3, magnesiumcarbonate 0.2, attapulgite 4, nano titanium oxide 1, accelerant CZ 0.05, dioctyl phthalate (DOP) 2, hexachlorocyclopentadiene 9, to toluene diisocyanate 2, antioxidant 2246 0.3, suitable quantity of water.
Making method comprises the following steps:
(1) white carbon black, urea, accelerant CZ 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, nano titanium oxide 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 attapulgite, dioctyl phthalate (DOP), hexachlorocyclopentadiene 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 92.1%;
The high thermal stability of (2) 105 DEG C/15min is the high thermal stability of 87%, 120 DEG C/15min is 53%.
Claims (3)
1. a weather-proof anti-aging high-thermostability insoluble sulfur, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.5-1.2, urea 0.2-0.4, magnesiumcarbonate 0.1-0.3, attapulgite 4-7, nano titanium oxide 1-2, accelerant CZ 0.03-0.07, dioctyl phthalate (DOP) 2-3, hexachlorocyclopentadiene 6-9, to toluene diisocyanate 2-4, antioxidant 2246 0.3-0.5, suitable quantity of water.
2. the making method of a kind of weather-proof anti-aging high-thermostability insoluble sulfur according to claim 1, is characterized in that comprising the following steps:
(1) white carbon black, urea, accelerant CZ 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, nano titanium oxide 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 attapulgite, dioctyl phthalate (DOP), hexachlorocyclopentadiene 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 weather-proof anti-aging high-thermostability insoluble sulfur 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 |
|---|---|---|---|
| CN201510071511.7A CN104671215A (en) | 2015-02-11 | 2015-02-11 | Weather-proof anti-aging high-thermal-stability insoluble sulfur and production method thereof |
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| CN201510071511.7A CN104671215A (en) | 2015-02-11 | 2015-02-11 | Weather-proof anti-aging high-thermal-stability insoluble sulfur and production method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542245A (en) * | 2016-01-22 | 2016-05-04 | 上海京海（安徽）化工有限公司 | High-performance rubber produced through rubber refining of high-thermal-stability insoluble sulfur and preparation method |
| CN105752941A (en) * | 2016-01-22 | 2016-07-13 | 上海京海（安徽）化工有限公司 | Method for preparing high-purity and high-dispersibility insoluble sulfur |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204479A (en) * | 2013-03-22 | 2013-07-17 | 上海京海（安徽）化工有限公司 | Production method for high-content insoluble sulfur |
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2015
- 2015-02-11 CN CN201510071511.7A patent/CN104671215A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204479A (en) * | 2013-03-22 | 2013-07-17 | 上海京海（安徽）化工有限公司 | Production method for high-content insoluble sulfur |
Non-Patent Citations (1)
| Title |
|---|
| 孙玉泉: "不溶性硫磺低温液相法制备工艺条件优化", 《化学工程师》, no. 11, 31 December 2011 (2011-12-31), pages 49 - 53 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542245A (en) * | 2016-01-22 | 2016-05-04 | 上海京海（安徽）化工有限公司 | High-performance rubber produced through rubber refining of high-thermal-stability insoluble sulfur and preparation method |
| CN105752941A (en) * | 2016-01-22 | 2016-07-13 | 上海京海（安徽）化工有限公司 | Method for preparing high-purity and high-dispersibility insoluble sulfur |
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Application publication date: 20150603 |
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