CN104671217A - Nano boron fibre/glass fibre composite insoluble sulfur and preparation method thereof - Google Patents
Nano boron fibre/glass fibre composite insoluble sulfur and preparation method thereof Download PDFInfo
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- CN104671217A CN104671217A CN201510071567.2A CN201510071567A CN104671217A CN 104671217 A CN104671217 A CN 104671217A CN 201510071567 A CN201510071567 A CN 201510071567A CN 104671217 A CN104671217 A CN 104671217A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/06—Sulfur
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2255—Oxides; Hydroxides of metals of molybdenum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
- C08K2003/3081—Aluminum sulfate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses nano boron fibre/glass fibre composite insoluble sulfur which is characterized by being prepared from the following raw materials in parts by weight: 100 parts of sulfur powder, 0.7-1.6 parts of white carbon black, 0.1-0.3 part of stainless steel powder, 0.04-0.08 part of sodium dodecyl benzene sulfonate, 1-3 parts of sorbitol anhydride stearate, 4-7 parts of paraffin oil, 0.5-0.8 part of nano boron fibre, 0.7-1.2 parts of glass fibre, 0.04-0.06 part of sodium persulfate, 0.2-0.4 part of molybdenum trioxide, 0.3-0.5 part of aluminum sulfate, 0.03-0.07 part of 2-mercaptobenzothiazole and a proper amount of water. The nano boron fibre/glass fibre composite insoluble sulfur is high in operation safety, low in toxicity, high in production efficiency and easy for industrialization; according to a low-temperature liquid-phase method, modified white carbon black is added as an antistatic agent during the preparation process, so that static electricity of a product is eliminated and the content of insoluble sulfur is increased; meanwhile, 0.1% pentaerythritol water solution is selected as quenching liquid, and has the characteristics of low cost, remarkable quenching effect and high quenching efficiency; nano boron fibre and glass fibre are added and composited with each other, so that the heat resistance, corrosion resistance, elasticity and mechanical strength of a rubber product are improved; and the prepared insoluble sulfur has high stability and good dispersibility.
Description
Technical field
The present invention relates to insoluble sulfur preparing technical field, be specifically related to insoluble sulfur of a kind of nanometer boron fibre/glass fibre compound 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 insoluble sulfur of a kind of nanometer boron fibre/glass fibre compound 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 insoluble sulfur of nanometer boron fibre/glass fibre compound, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.7-1.6, Stainless Steel Powder 0.1-0.3, Sodium dodecylbenzene sulfonate 0.04-0.08, sorbitan tristearate 1-3, paraffin oil 4-7, nanometer boron fibre 0.5-0.8, glass fibre 0.7-1.2, Sodium Persulfate 0.04-0.06, molybdic oxide 0.2-0.4, Tai-Ace S 150 0.3-0.5,2-thiol group benzimidazolyl 0.03-0.07, suitable quantity of water.
The preparation method of the insoluble sulfur of described a kind of nanometer boron fibre/glass fibre compound, is characterized in that comprising the following steps:
(1) Stainless Steel Powder after white carbon black, Sodium dodecylbenzene sulfonate and gelatinization process is 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 160 DEG C and adds modified white carbon black, nanometer boron fibre, glass fibre, molybdic oxide mixing, continue to be warming up to 220-300 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 sorbitan tristearate, paraffin 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: processing safety of the present invention is high, toxicity is little, production efficiency is high, be easy to industrialization, 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, there is cost low, quenching Be very effective, the feature that extraction efficiency is high, also add nanometer boron fibre and the mutual compound of glass fibre, the thermotolerance of rubber product can be improved, erosion resistance, elasticity and physical strength, the insoluble sulfur stability preparing gained is high, good dispersity.
Embodiment
The insoluble sulfur of described a kind of nanometer boron fibre/glass fibre compound, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.9, Stainless Steel Powder 0.2, Sodium dodecylbenzene sulfonate 0.06, sorbitan tristearate 1, paraffin oil 4, nanometer boron fibre 0.7, glass fibre 1.2, Sodium Persulfate 0.05, molybdic oxide 0.2, Tai-Ace S 150 0.3,2-thiol group benzimidazolyl 0.04, suitable quantity of water.
Making method comprises the following steps:
(1) Stainless Steel Powder after white carbon black, Sodium dodecylbenzene sulfonate and gelatinization process is 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 160 DEG C and adds modified white carbon black, nanometer boron fibre, glass fibre, molybdic oxide mixing, continue to be warming up to 220-300 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 sorbitan tristearate, paraffin 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 86.5%;
(2) the oil-filled type insoluble sulfur performance index prepared are better than chemical industry standard HG/T2525-93, and product high-temperature stability reaches 91.8 %.
Claims (3)
1. the insoluble sulfur of nanometer boron fibre/glass fibre compound, it is characterized in that, be made up of the raw material of following weight part: SULPHUR POWDER 100, white carbon black 0.7-1.6, Stainless Steel Powder 0.1-0.3, Sodium dodecylbenzene sulfonate 0.04-0.08, sorbitan tristearate 1-3, paraffin oil 4-7, nanometer boron fibre 0.5-0.8, glass fibre 0.7-1.2, Sodium Persulfate 0.04-0.06, molybdic oxide 0.2-0.4, Tai-Ace S 150 0.3-0.5,2-thiol group benzimidazolyl 0.03-0.07, suitable quantity of water.
2. the making method of the insoluble sulfur of a kind of nanometer boron fibre/glass fibre compound according to claim 1, is characterized in that comprising the following steps:
(1) Stainless Steel Powder after white carbon black, Sodium dodecylbenzene sulfonate and gelatinization process is 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 160 DEG C and adds modified white carbon black, nanometer boron fibre, glass fibre, molybdic oxide mixing, continue to be warming up to 220-300 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 sorbitan tristearate, paraffin 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 insoluble sulfur of a kind of nanometer boron fibre/glass fibre compound 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 |
|---|---|---|---|
| CN201510071567.2A CN104671217A (en) | 2015-02-11 | 2015-02-11 | Nano boron fibre/glass fibre composite insoluble sulfur and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510071567.2A CN104671217A (en) | 2015-02-11 | 2015-02-11 | Nano boron fibre/glass fibre composite insoluble sulfur and preparation method thereof |
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| CN104671217A true CN104671217A (en) | 2015-06-03 |
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| CN201510071567.2A Pending CN104671217A (en) | 2015-02-11 | 2015-02-11 | Nano boron fibre/glass fibre composite insoluble sulfur and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964645A (en) * | 2012-11-29 | 2013-03-13 | 泰亚鞋业股份有限公司 | Ice surface anti-slip rubber sports shoe soles and manufacturing method thereof |
| 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 |
-
2015
- 2015-02-11 CN CN201510071567.2A patent/CN104671217A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964645A (en) * | 2012-11-29 | 2013-03-13 | 泰亚鞋业股份有限公司 | Ice surface anti-slip rubber sports shoe soles and manufacturing method thereof |
| 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", 《精细化工原料及中间体》, no. 3, 31 December 2010 (2010-12-31), pages 19 - 23 * |
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