CN107987318A - A kind of novel metal reinforcing agent as rubber processing - Google Patents
A kind of novel metal reinforcing agent as rubber processing Download PDFInfo
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- CN107987318A CN107987318A CN201711410656.0A CN201711410656A CN107987318A CN 107987318 A CN107987318 A CN 107987318A CN 201711410656 A CN201711410656 A CN 201711410656A CN 107987318 A CN107987318 A CN 107987318A
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
- C08L21/00—Compositions of unspecified rubbers
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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
- C08K2003/3009—Sulfides
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- Health & Medical Sciences (AREA)
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention relates to novel metal functional material research and development technology field,Disclose a kind of novel metal reinforcing agent as rubber processing,Molybdenum disulfide is carried out structurally-modified,Improve the compatibility with rubber,As rubber reinforcing filler,Dosage is few,Only add the product that mass fraction is 0.01%,80% and 70% has just been respectively increased in the modulus and tensile strength of elastomeric material,And compression heat generation value reduces 20 DEG C,It is notable to the enhancing effect of rubber,Durability is grown,The mechanical property of elastomeric material can be significantly improved,Improve the wearability and anti-slippery of rubber,And the metal material for coating organic matter is obviously improved for the absorption of ultraviolet,Ageing resistance obtains certain enhancing,The metal reinforcement agent that the present invention is prepared is very notable to improving the scattered humidification of metal and metallic compound in rubber matrix,It is of great significance for preparing high-performance rubber composite material.
Description
Technical field
The invention belongs to novel metal functional material research and development technology field, and in particular to a kind of to be used as what rubber was processed
Novel metal reinforcing agent.
Background technology
Rubber is the high-molecular compound for having at room temperature viscoelasticity, and various rubbers are can be made into by vulcanization reaction,
With plastics, fiber and claiming modern three big high molecular materials.The usage history of rubber can trace back to for 11st century, and south American is at first
It was found that and it is made into ball, rubber bottle, rubber boots using the high resiliency of rubber.Hereafter, with vulcanizer, the hair of twin-roll machine
Bright, the application of rubber has obtained further development.However, since rubber molecule intermolecular forces are small, crystal energy force difference, cause rubber
The modulus of product, intensity, fatigue behaviour cannot meet application request.Therefore, most of rubber need to carry out using filler
Reinforcement, to improve the performance of rubber.Traditional rubber reinforcing filler has carbon black, white carbon, clay etc., these fillers can improve
The tensile strength of rubber, tearing strength, wearability etc., dosage is generally more than ten parts to tens parts, and dosage is very big, but durability one
As.
With the continuous development of scientific technology, metal nanoparticle and the composite material that is prepared into by it it is metallurgical,
The research fields such as chemical industry light industry electronics national defence, nuclear technology, aerospace show extremely important application value.Novel nano material
Expect such as carbon nanotubes, graphene, there is the characteristics such as intensity is high, specific surface area is big also can effectively strengthen rubber, but itself and rubber
Affinity it is poor, easily disintegrate under mechanical force.
The content of the invention
The purpose of the present invention is for it is existing the problem of, there is provided it is a kind of as rubber processing novel metal reinforcement
Agent, dosage is few, notable to the enhancing effect of rubber, and durability length, improves the compatibility with rubber.
The present invention is achieved by the following technical solutions：
A kind of novel metal reinforcing agent as rubber processing, prepares synthetic method and comprises the following steps：
（1）Weigh 0.20-0.23 moles of molybdenum disulfide powder dry 10-12 in 80-85 DEG C of air dry oven it is small when, add
Into three-necked flask, and nitrogen is passed through to eliminate the air in three-necked flask, it is 10-15% then to add 40-50 milliliters of concentration
N-BuLi add in flask, under nitrogen atmosphere protection with 300-350 revs/min of mixing speed at 50-60 DEG C it is anti-
When answering 6-8 small, after reaction, filtered, the product of suction filtration is transferred in 180-200 ml deionized waters, at ultrasound
Reason 15-20 minutes, finally, molybdenum disulfide aqueous solution is centrifuged 2-3 times, removes supernatant, in 70-80 DEG C of vacuum
Pulverize when drying 6-8 is small in drying box spare；
（2）10-12 milliliters of tetrahydrofurans are added in flask, adding 0.14-0.16 grams under nitrogen atmosphere protection does not aoxidize
Sodium piece and 0.3-0.4 grams of benzophenone, 120-130 DEG C heating under flow back, be back to solution colour and be changed into navy blue
Afterwards, device is changed to distilling apparatus, distilled under normal pressure 1.5-2.0 it is small when, vapo(u)rizing temperature control is distilled in 90-95 DEG C of scope
Liquid is spare；
（3）By step（1）The powder and step being prepared（2）The distillate mixing being prepared, adds 30-35 milliliters of second two
Amine, ultrasonic disperse 10-15 minutes, by 4.5-5.5 grams of anhydrous cupric sulfate and 2.5-3.0 grams of sodium bromide be dissolved in 40-50 milliliters go from
In sub- water, 8-10 milliliters of hypo solutions are added under continuous stirring, are added dropwise in 7-9 minutes, obtained mixing
Liquid is stirred with ethylenediamine system, is added in reaction kettle, at 180-190 DEG C react 15-18 it is small when, obtain reactant into
Row is filtered, washed, being drying to obtain the metal reinforcement agent.
Further described as to such scheme, step（1）The concentration is that the n-BuLi of 10-15% is dissolved in
Concentration is the hexane solution of 1.0-1.2 mol/Ls.
Further described as to such scheme, step（1）The centrifugation rotating speed is 4000-4200 revs/min.
Further described as to such scheme, step（3）The preparation method of the hypo solution is：
At 35-45 DEG C, 2-3 grams of sodium thiosulfate is added in 25-30 ml deionized waters stirring and dissolving 30-40 minutes.
The present invention has the following advantages compared with prior art：It is poor with rubber compatibility in order to solve existing gum filler, use
The problem of amount is more, and durability is poor, the present invention provides a kind of novel metal reinforcing agent as rubber processing, to curing
Molybdenum progress is structurally-modified, improves the compatibility with rubber, and as rubber reinforcing filler, dosage is few, only adds mass fraction and is
0.01% product, 80% and 70% has just been respectively increased in the modulus and tensile strength of elastomeric material, and compression heat generation value reduces
20 DEG C, notable to the enhancing effect of rubber, durability length, can significantly improve the mechanical property of elastomeric material, improve rubber
The wearability and anti-slippery of product, and the metal material for coating organic matter is obviously improved for the absorption of ultraviolet,
Ageing resistance obtains certain enhancing, and the metal reinforcement agent that the present invention is prepared is to improving metal and metallic compound in rubber
Scattered humidification in matrix body is very notable, is of great significance for preparing high-performance rubber composite material.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
A kind of novel metal reinforcing agent as rubber processing, prepares synthetic method and comprises the following steps：
（1）Weigh 0.20 mole of molybdenum disulfide powder in 80 DEG C of air dry ovens it is dry 10 it is small when, be added in three-necked flask,
And nitrogen is passed through to eliminate the air in three-necked flask, then add the n-BuLi that 40 milliliters of concentration are 10% and add flask
In, reacted under nitrogen atmosphere protection at 50 DEG C with 300 revs/min of mixing speed 6 it is small when, after reaction, taken out
Filter, the product of suction filtration is transferred in 180 ml deionized waters, be ultrasonically treated 15 minutes, finally, by molybdenum disulfide aqueous solution into
Row centrifuges 2 times, removes supernatant, pulverizes when drying 6 is small in 70 DEG C of vacuum drying chambers spare；
（2）10 milliliters of tetrahydrofurans are added in flask, added under nitrogen atmosphere protection 0.14 gram of unoxidized sodium piece and
0.3 gram of benzophenone, flows back under 120 DEG C of heating, is back to after solution colour is changed into navy blue, device is changed to distillation dress
Put, when distillation 1.5 is small under normal pressure, vapo(u)rizing temperature is controlled in 90-95 DEG C of scope, and it is spare to obtain distillate；
（3）By step（1）The powder and step being prepared（2）The distillate mixing being prepared, adds 30 milliliters of ethylenediamines,
Ultrasonic disperse 10 minutes, 4.5 grams of anhydrous cupric sulfates and 2.5 grams of sodium bromides are dissolved in 40 ml deionized waters, are constantly being stirred
8 milliliters of hypo solutions of lower addition to be mixed, are added dropwise in 7 minutes, obtained mixed liquor is stirred with ethylenediamine system,
It is added in reaction kettle, when reaction 15 is small at 180 DEG C, obtains reactant and filtered, washed, being drying to obtain the metal benefit
Strong agent.
Further described as to such scheme, step（1）The n-BuLi that the concentration is 10% is dissolved in concentration
For the hexane solution of 1.0 mol/Ls.
Further described as to such scheme, step（1）The centrifugation rotating speed is 4000 revs/min.
Further described as to such scheme, step（3）The preparation method of the hypo solution is：35
At DEG C, 2 grams of sodium thiosulfate is added to stirring and dissolving 30 minutes in 25 ml deionized waters.
Embodiment 2
A kind of novel metal reinforcing agent as rubber processing, prepares synthetic method and comprises the following steps：
（1）Weigh 0.22 mole of molybdenum disulfide powder in 82 DEG C of air dry ovens it is dry 11 it is small when, be added in three-necked flask,
And nitrogen is passed through to eliminate the air in three-necked flask, then add the n-BuLi that 45 milliliters of concentration are 12% and add flask
In, reacted under nitrogen atmosphere protection at 54 DEG C with 330 revs/min of mixing speed 7 it is small when, after reaction, taken out
Filter, the product of suction filtration is transferred in 190 ml deionized waters, be ultrasonically treated 18 minutes, finally, by molybdenum disulfide aqueous solution into
Row centrifuges 2 times, removes supernatant, pulverizes when drying 7 is small in 75 DEG C of vacuum drying chambers spare；
（2）10-12 milliliters of tetrahydrofurans are added in flask, 0.15 gram of unoxidized sodium piece is added under nitrogen atmosphere protection
With 0.35 gram of benzophenone, flow back, be back to after solution colour is changed into navy blue, device is changed to steaming under 125 DEG C of heating
Distillation unit, when distillation 1.8 is small under normal pressure, it is spare to obtain distillate in 90-95 DEG C of scope for vapo(u)rizing temperature control；
（3）By step（1）The powder and step being prepared（2）The distillate mixing being prepared, adds 32 milliliters of ethylenediamines,
Ultrasonic disperse 12 minutes, 5.0 grams of anhydrous cupric sulfates and 2.8 grams of sodium bromides are dissolved in 45 ml deionized waters, are constantly being stirred
9 milliliters of hypo solutions of lower addition to be mixed, are added dropwise in 8 minutes, obtained mixed liquor is stirred with ethylenediamine system,
It is added in reaction kettle, when reaction 16 is small at 185 DEG C, obtains reactant and filtered, washed, being drying to obtain the metal benefit
Strong agent.
Further described as to such scheme, step（1）The n-BuLi that the concentration is 12% is dissolved in concentration
For the hexane solution of 1.1 mol/Ls.
Further described as to such scheme, step（1）The centrifugation rotating speed is 4100 revs/min.
Further described as to such scheme, step（3）The preparation method of the hypo solution is：40
At DEG C, 2.5 grams of sodium thiosulfate is added to stirring and dissolving 35 minutes in 28 ml deionized waters.
Embodiment 3
A kind of novel metal reinforcing agent as rubber processing, prepares synthetic method and comprises the following steps：
（1）Weigh 0.23 mole of molybdenum disulfide powder in 85 DEG C of air dry ovens it is dry 12 it is small when, be added to three-necked flask
In, and nitrogen is passed through to eliminate the air in three-necked flask, then add the n-BuLi that 50 milliliters of concentration are 15% and add and burn
In bottle, react under nitrogen atmosphere protection at 60 DEG C with 350 revs/min of mixing speed 8 it is small when, after reaction, progress
Filter, the product of suction filtration is transferred in 200 ml deionized waters, be ultrasonically treated 20 minutes, finally, by molybdenum disulfide aqueous solution
It is centrifuged 3 times, removes supernatant, pulverizes when drying 8 is small in 80 DEG C of vacuum drying chambers spare；
（2）12 milliliters of tetrahydrofurans are added in flask, added under nitrogen atmosphere protection 0.16 gram of unoxidized sodium piece and
0.4 gram of benzophenone, flows back under 130 DEG C of heating, is back to after solution colour is changed into navy blue, device is changed to distillation dress
Put, when distillation 2.0 is small under normal pressure, vapo(u)rizing temperature is controlled in 90-95 DEG C of scope, and it is spare to obtain distillate；
（3）By step（1）The powder and step being prepared（2）The distillate mixing being prepared, adds 35 milliliters of ethylenediamines,
Ultrasonic disperse 15 minutes, 5.5 grams of anhydrous cupric sulfates and 3.0 grams of sodium bromides are dissolved in 50 ml deionized waters, are constantly being stirred
10 milliliters of hypo solutions of lower addition are mixed, are added dropwise in 9 minutes, obtained mixed liquor and the stirring of ethylenediamine system are mixed
Close, be added in reaction kettle, when reaction 18 is small at 190 DEG C, obtains reactant and filtered, washed, being drying to obtain the gold
Belong to reinforcing agent.
Further described as to such scheme, step（1）The n-BuLi that the concentration is 15% is dissolved in concentration
For the hexane solution of 1.2 mol/Ls.
Further described as to such scheme, step（1）The centrifugation rotating speed is 4200 revs/min.
Further described as to such scheme, step（3）The preparation method of the hypo solution is：45
At DEG C, 3 grams of sodium thiosulfate is added to stirring and dissolving 40 minutes in 30 ml deionized waters.
Claims (4)
1. a kind of novel metal reinforcing agent as rubber processing, it is characterised in that preparing synthetic method includes following step
Suddenly：
（1）Weigh 0.20-0.23 moles of molybdenum disulfide powder dry 10-12 in 80-85 DEG C of air dry oven it is small when, add
Into three-necked flask, and nitrogen is passed through to eliminate the air in three-necked flask, it is 10-15% then to add 40-50 milliliters of concentration
N-BuLi add in flask, under nitrogen atmosphere protection with 300-350 revs/min of mixing speed at 50-60 DEG C it is anti-
When answering 6-8 small, after reaction, filtered, the product of suction filtration is transferred in 180-200 ml deionized waters, at ultrasound
Reason 15-20 minutes, finally, molybdenum disulfide aqueous solution is centrifuged 2-3 times, removes supernatant, in 70-80 DEG C of vacuum
Pulverize when drying 6-8 is small in drying box spare；
（2）10-12 milliliters of tetrahydrofurans are added in flask, adding 0.14-0.16 grams under nitrogen atmosphere protection does not aoxidize
Sodium piece and 0.3-0.4 grams of benzophenone, 120-130 DEG C heating under flow back, be back to solution colour and be changed into navy blue
Afterwards, device is changed to distilling apparatus, distilled under normal pressure 1.5-2.0 it is small when, vapo(u)rizing temperature control is distilled in 90-95 DEG C of scope
Liquid is spare；
（3）By step（1）The powder and step being prepared（2）The distillate mixing being prepared, adds 30-35 milliliters of second two
Amine, ultrasonic disperse 10-15 minutes, by 4.5-5.5 grams of anhydrous cupric sulfate and 2.5-3.0 grams of sodium bromide be dissolved in 40-50 milliliters go from
In sub- water, 8-10 milliliters of hypo solutions are added under continuous stirring, are added dropwise in 7-9 minutes, obtained mixing
Liquid is stirred with ethylenediamine system, is added in reaction kettle, at 180-190 DEG C react 15-18 it is small when, obtain reactant into
Row is filtered, washed, being drying to obtain the metal reinforcement agent.
A kind of 2. novel metal reinforcing agent as rubber processing as claimed in claim 1, it is characterised in that step（1）
The n-BuLi that the concentration is 10-15% is dissolved in the hexane solution that concentration is 1.0-1.2 mol/Ls.
A kind of 3. novel metal reinforcing agent as rubber processing as claimed in claim 1, it is characterised in that step（1）
The centrifugation rotating speed is 4000-4200 revs/min.
A kind of 4. novel metal reinforcing agent as rubber processing as claimed in claim 1, it is characterised in that step（3）
The preparation method of the hypo solution is：At 35-45 DEG C, 2-3 grams of sodium thiosulfate is added to 25-30 milliliters
Stirring and dissolving 30-40 minutes in deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711410656.0A CN107987318A (en) | 2017-12-23 | 2017-12-23 | A kind of novel metal reinforcing agent as rubber processing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711410656.0A CN107987318A (en) | 2017-12-23 | 2017-12-23 | A kind of novel metal reinforcing agent as rubber processing |
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| Publication Number | Publication Date |
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| CN107987318A true CN107987318A (en) | 2018-05-04 |
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| CN201711410656.0A Pending CN107987318A (en) | 2017-12-23 | 2017-12-23 | A kind of novel metal reinforcing agent as rubber processing |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024516A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | (NH4+)XMOS2 intercalation compound and its preparing method |
| CN102101696A (en) * | 2010-12-02 | 2011-06-22 | 华东师范大学 | Preparation method of ethanediamine intercalation tin sulfide compound |
| CN103275355A (en) * | 2013-05-20 | 2013-09-04 | 中国科学技术大学 | Organic modified molybdenum disulfide nanosheet layer and preparation method thereof |
| CN104310482A (en) * | 2014-09-29 | 2015-01-28 | 南京邮电大学 | Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation |
| CN106564953A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for reducing preparation of graphene-like molybdenum disulfide through carbohydrate organic carbon |
-
2017
- 2017-12-23 CN CN201711410656.0A patent/CN107987318A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024516A (en) * | 2007-01-30 | 2007-08-29 | 合肥工业大学 | (NH4+)XMOS2 intercalation compound and its preparing method |
| CN102101696A (en) * | 2010-12-02 | 2011-06-22 | 华东师范大学 | Preparation method of ethanediamine intercalation tin sulfide compound |
| CN103275355A (en) * | 2013-05-20 | 2013-09-04 | 中国科学技术大学 | Organic modified molybdenum disulfide nanosheet layer and preparation method thereof |
| CN104310482A (en) * | 2014-09-29 | 2015-01-28 | 南京邮电大学 | Method for preparing molybdenum disulfide nanosheets by ultrasonic-assisted chemical intercalation |
| CN106564953A (en) * | 2016-11-04 | 2017-04-19 | 西安建筑科技大学 | Method for reducing preparation of graphene-like molybdenum disulfide through carbohydrate organic carbon |
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Application publication date: 20180504 |
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