CN107141524B - A kind of preparation method for the insulating rubber material that methylates - Google Patents
A kind of preparation method for the insulating rubber material that methylates Download PDFInfo
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- CN107141524B CN107141524B CN201710384695.1A CN201710384695A CN107141524B CN 107141524 B CN107141524 B CN 107141524B CN 201710384695 A CN201710384695 A CN 201710384695A CN 107141524 B CN107141524 B CN 107141524B
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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
- C08L7/00—Compositions of natural rubber
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Organic Chemistry (AREA)
- Organic Insulating Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods for the insulating rubber material that methylates, kaolin and elastomer are effectively combined, improve dispersiveness, the compatibility of filler, so as to improve the stability_intensity of finished-product material, the elastomer of addition has good buffering effect, can improve compression strength, the impact strength of finished product, the finished-product material insulation stability of the present invention is good, bin stability is high, and safety in utilization is good, and comprehensive performance is superior.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of preparation method for the insulating rubber material that methylates.
Background technology
Insulating materials can divide gas, liquid, solid three categories.Common gas insulating material has air, nitrogen, lithium
Sulphur etc..Liquid insulating material mainly has mineral insulating oil, synthetic insulating oil（Silicone oil, detergent alkylate, polyisobutene, isopropyl
Biphenyl, diarylethane etc.）Two classes.Solid insulating material can be divided to organic and inorganic two class.Organic solid insulating materials includes insulation
Paint, insulating cement, insulating paper, non-conductive fibre product, plastics, rubber, varnished cloth paint pipe and insulation impregnating fibre, electrician are with thin
Film, composite article and adhesive tape, electrician's laminated product etc..Inoganic solids insulating materials mainly has mica, glass, ceramics and its system
Product.In contrast, solid insulating material is numerous in variety, also mostly important.Different electrical equipments want insulating material properties
Ask and emphasize particularly on different fields, the requirement of the insulating materials of high pressure electrical device such as high-voltage motor, high-tension cable etc. have high breakdown strength and
Low dielectric loss.Low-voltage electrical apparatus is then using mechanical strength, elongation at break, temperature classification etc. as major requirement.
The macro property of insulating materials such as electrical property, hot property, mechanical property, chemical-resistant resistance, weatherability variation, corrosion resistant
The performances and its chemical composition, molecular structure etc. such as erosion have substantial connection.Inoganic solids insulating materials is mainly by silicon, boron and more
Kind metal oxide composition based on ionic structure, is mainly characterized in that heat resistance height, and operating temperature is generally higher than 180 DEG C surely
It is qualitative good, resistance to weathering, chemical resistance and the ageing properties under electric field action are good for a long time；But brittleness is high, resistance to punching
Hit intensity is low, high pressure and tensile strength is low；Craftsmanship is poor.Organic material is generally polymer, and heat resistance is usually less than nothing
Machine material.Material its heat resistance containing the elements such as aromatic ring, heterocycle and silicon, titanium, fluorine is then higher than general line chain high molecular material.
With the development of society, more and more electrical equipments enter in the family, factory, social environment of people, in order to
People’s lives more safety can be allowed, it is necessary to which the insulating materials that insulation effect is better, performance is more reliable is exhausted to meet electric appliance
The requirement of edge performance, and rubber material is often used in as electric appliance protective materials, however it is easily as common insulating materials
Aging, bin stability is poor, and the inorganic filler property compatible added is poor, greatly reduces the quality of finished product, reduces
Safety in utilization.
The content of the invention
It is an object of the invention to be directed to the easy to aging of natural rubber in the prior art, bin stability is poor, and add
The problem of inorganic filler property compatible is poor provides a kind of preparation method for the insulating rubber material that methylates.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method for the insulating rubber material that methylates, comprises the following steps：
（1）The polyamide wax micropowder of 1-3 parts by weight is taken, is added in the N-Methyl pyrrolidone of 7-10 parts by weight, is stirred
Uniformly, it is sent in 130-140 DEG C of oil bath, insulated and stirred 10-20 minutes, discharges, adds in the borax of 0.7-1 parts by weight, stir
It mixes to room temperature, obtains wax micro mist dispersion liquid；
（2）The 8-hydroxyquinoline of 1-2 parts by weight is taken, is added in the ethylene glycol of 18-20 times of its weight, stirs evenly；
（3）The kaolin of 13-20 parts by weight is taken, when calcining 1-2 is small at 700-800 DEG C, fine powder is worn into after cooling, is added in
When into the sulfuric acid solution of 10-13mol/L, immersion 3-5 is small, discharge, washing, air drying, the aluminum stearate with 1-2 parts by weight
It mixes, in carbon acid solution that be added to 3-4 times of mixture weight, 20-25%, 10-20 minutes ultrasonic, must organise kaolin
Dispersion liquid；
（4）The kaolin dispersion liquid that organises is taken, mixes, stirs evenly with the ethylene glycol solution of 8-hydroxyquinoline, be sent to
In ptfe autoclave, when insulation reaction 1-2 is small at 90-100 DEG C, discharge, dehydration, air drying obtains esterification kaolinite
Soil；
（5）The stannous octoate mixing of above-mentioned esterification kaolin, 0.2-0.4 parts by weight is taken, above-mentioned wax micro mist is added to and disperses
It in liquid, stirs evenly, kaolin micro mist dispersion liquid must be esterified；
（6）The formamide mixing of the SIS thermoplastic elastomer (TPE)s, 2-3 parts by weight of 27-30 parts by weight is taken, is added to mixture
In the absolute ethyl alcohol of 1.6-2 times of weight, when insulated and stirred 1-2 is small at 60-65 DEG C, ethyl alcohol is distilled off, obtains amination elastomer；
（7）Above-mentioned esterification kaolin micro mist dispersion liquid, the mixing of amination elastomer are taken, stirs evenly, 18-20 parts by weight is added dropwise
, concentration be 10-14% formalin, rise temperature be 60-70 DEG C, insulated and stirred 100-110 minutes is cooled to room temperature, obtains
Methylate kaolin elastomer solution；
（8）The above-mentioned kaolin elastomer solution that methylates is taken, the natural rubber, 4-5 parts by weight with 200-300 parts by weight
Anti-aging agent rd is mixed, and is sent into mixer, mixing 30-40s, and mixing temperature is 60-100 DEG C, adds in the chlorination of 20-34 parts by weight
Paraffin is kneaded 6-8 minutes, dumping, is cooled to 20-30 DEG C, is put into open mill, adds in zinc oxide, the 2.8- of 0.7-1 parts by weight
The sulphur of 3 parts by weight, the captax BS, thin logical 3-5 of 3-4 parts by weight are all over to get the insulating rubber material that methylates.
Advantages of the present invention：
The present invention uses polyamide wax micropowder as raw material first, disperses in pyrrolidones, obtains wax micro mist dispersion liquid, together
When add in borax, improve the surface strength of micro mist, it is then that the ethylene glycol solution of 8-hydroxyquinoline and kaolinic carbonic acid is molten
Liquid hybrid reaction obtains carbonic ester kaolin, while when kaolin is distributed to carbon acid solution, it will using aluminum stearate
Activation of kaoline improves the kaolinic forming stability of carbonic ester, and then thermoplastic elastomer (TPE) is handled using formamide, is obtained
To amidated elastomer, then mixed with formalin, it, can be with by the cross-linking reaction of formalin and amidation elastomer
Methylolated elastomer is obtained, and while reaction, esterification kaolin micro mist dispersion liquid is also introduced, dimethyl carbonate is also
Can be used as and methylate auxiliary agent, improve the cross-link intensity of formalin and amidation elastomer, at the same by kaolin with it is elastic
Body is effectively combined, and improves dispersiveness, the compatibility of filler, so as to improve the stability_intensity of finished-product material, addition
Elastomer has good buffering effect, can improve compression strength, the impact strength of finished product, and finished-product material of the invention is exhausted
Edge stability is good, and bin stability is high, and safety in utilization is good, and comprehensive performance is superior.
Specific embodiment
Embodiment 1
A kind of preparation method for the insulating rubber material that methylates, comprises the following steps：
（1）The polyamide wax micropowder of 3 parts by weight is taken, is added in the N-Methyl pyrrolidone of 10 parts by weight, stirs evenly,
It is sent in 140 DEG C of oil bath, insulated and stirred 20 minutes, discharges, add in the borax of 1 parts by weight, stir to room temperature, obtain wax micro mist
Dispersion liquid；
（2）The 8-hydroxyquinoline of 2 parts by weight is taken, is added in the ethylene glycol of 20 times of its weight, stirs evenly；
（3）The kaolin of 20 parts by weight is taken, when calcining 2 is small at 800 DEG C, fine powder is worn into after cooling, adds in 13mol/L
Sulfuric acid solution in impregnate 5 it is small when, discharge, washing, air drying mixes with the aluminum stearate of 2 parts by weight, be added to mixture
In 4 times of weight, 25% carbon acid solution, ultrasound 20 minutes, must organise kaolin dispersion liquid；
（4）The kaolin dispersion liquid that organises is taken, mixes, stirs evenly with the ethylene glycol solution of 8-hydroxyquinoline, be sent to
In ptfe autoclave, when insulation reaction 2 is small at 100 DEG C, discharge, dehydration, air drying obtains esterification kaolin；
（5）The stannous octoate mixing of above-mentioned esterification kaolin, 0.4 parts by weight is taken, is added in above-mentioned wax micro mist dispersion liquid,
It stirs evenly, kaolin micro mist dispersion liquid must be esterified；
（6）The formamide mixing of the SIS thermoplastic elastomer (TPE)s, 3 parts by weight of 30 parts by weight is taken, is added to mixture weight 2
In absolute ethyl alcohol again, when insulated and stirred 2 is small at 65 DEG C, ethyl alcohol is distilled off, obtains amination elastomer；
（7）Above-mentioned esterification kaolin micro mist dispersion liquid, the mixing of amination elastomer are taken, is stirred evenly, 20 parts by weight of dropwise addition,
Concentration is 14% formalin, and rise temperature is 70 DEG C, and insulated and stirred 110 minutes is cooled to room temperature, and must methylate kaolin
Elastomer solution；
（8）The above-mentioned kaolin elastomer solution that methylates is taken, natural rubber, the anti-aging agent of 5 parts by weight with 300 parts by weight
Rd is mixed, and is sent into mixer, mixing 40s, and mixing temperature is 100 DEG C, is added in the chlorinated paraffin of 34 parts by weight, is kneaded 8 minutes,
Dumping is cooled to 30 DEG C, puts into open mill, the promotion of the zinc oxide of 1 parts by weight of addition, the sulphur, 4 parts by weight of 3 parts by weight
Agent MBS, thin logical 5 times to get the insulating rubber material that methylates.
Embodiment 2
A kind of preparation method for the insulating rubber material that methylates, comprises the following steps：
（1）The polyamide wax micropowder of 1 parts by weight is taken, is added in the N-Methyl pyrrolidone of 7 parts by weight, stirs evenly,
It is sent in 130 DEG C of oil bath, insulated and stirred 10 minutes, discharges, add in the borax of 0.7 parts by weight, stir to room temperature, it is micro- to obtain wax
Powder dispersion liquid；
（2）The 8-hydroxyquinoline of 1 parts by weight is taken, is added in the ethylene glycol of 18 times of its weight, stirs evenly；
（3）The kaolin of 13 parts by weight is taken, when calcining 1 is small at 700 DEG C, fine powder is worn into after cooling, is added to 10mol/L
Sulfuric acid solution in impregnate 3 it is small when, discharge, washing, air drying mixes with the aluminum stearate of 1 parts by weight, be added to mixture
In 3 times of weight, 20% carbon acid solution, ultrasound 10 minutes, must organise kaolin dispersion liquid；
（4）The kaolin dispersion liquid that organises is taken, mixes, stirs evenly with the ethylene glycol solution of 8-hydroxyquinoline, be sent to
In ptfe autoclave, when insulation reaction 1 is small at 90 DEG C, discharge, dehydration, air drying obtains esterification kaolin；
（5）The stannous octoate mixing of above-mentioned esterification kaolin, 0.2 parts by weight is taken, is added in above-mentioned wax micro mist dispersion liquid,
It stirs evenly, kaolin micro mist dispersion liquid must be esterified；
（6）The formamide mixing of the SIS thermoplastic elastomer (TPE)s, 2 parts by weight of 27 parts by weight is taken, is added to mixture weight
In 1.6 times of absolute ethyl alcohol, when insulated and stirred 1 is small at 60 DEG C, ethyl alcohol is distilled off, obtains amination elastomer；
（7）Above-mentioned esterification kaolin micro mist dispersion liquid, the mixing of amination elastomer are taken, is stirred evenly, 18 parts by weight of dropwise addition,
Concentration is 10% formalin, and rise temperature is 60 DEG C, and insulated and stirred 100 minutes is cooled to room temperature, and must methylate kaolin
Elastomer solution；
（8）The above-mentioned kaolin elastomer solution that methylates is taken, natural rubber, the anti-aging agent of 4 parts by weight with 200 parts by weight
Rd is mixed, and is sent into mixer, mixing 30s, and mixing temperature is 60 DEG C, is added in the chlorinated paraffin of 20-34 parts by weight, is kneaded 6 points
Clock, dumping are cooled to 20 DEG C, put into open mill, add in the zinc oxide of 0.7 parts by weight, the sulphur of 2.8 parts by weight, 3 parts by weight
Captax BS, thin logical 3 times to get the insulating rubber material that methylates.
Performance test：
The resistivity of material of the present invention is（7-9）×1015-16Ω·cm；
Bending strength is 120.4-130.6MPa；
Compressive strength is 133.1-142.5MPa；
Parallel layers to breakdown voltage be 30-45KV；
The resistivity of traditional natural rubber material is（1-4）×1013-14Ω·cm；
Bending strength is 102.3-105MPa；
Compressive strength is 100.7-108MPa；
Parallel layers to breakdown voltage be 10-15KV.
As can be seen that the insulating rubber material that methylates of the present invention is with higher insulating properties, bending strength, compressive strength
With anti-breakdown voltage, comprehensive performance is stronger, safety in utilization higher.
Claims (1)
1. a kind of preparation method for the insulating rubber material that methylates, which is characterized in that comprise the following steps：
（1）The polyamide wax micropowder of 1-3 parts by weight is taken, is added in the N-Methyl pyrrolidone of 7-10 parts by weight, stirs evenly,
It is sent in 130-140 DEG C of oil bath, insulated and stirred 10-20 minutes, discharges, add in the borax of 0.7-1 parts by weight, stir to normal
Temperature obtains wax micro mist dispersion liquid；
（2）The 8-hydroxyquinoline of 1-2 parts by weight is taken, is added in the ethylene glycol of 18-20 times of its weight, stirs evenly；
（3）The kaolin of 13-20 parts by weight is taken, when calcining 1-2 is small at 700-800 DEG C, fine powder is worn into after cooling, is added to
It when immersion 3-5 is small in the sulfuric acid solution of 10-13mol/L, discharges, washing, air drying is mixed with the aluminum stearate of 1-2 parts by weight
It closes, 10-20 minutes ultrasonic in carbon acid solution that be added to 3-4 times of mixture weight, 20-25%, the kaolin that must organise point
Dispersion liquid；
（4）The kaolin dispersion liquid that organises is taken, mixes, stirs evenly with the ethylene glycol solution of 8-hydroxyquinoline, is sent to poly- four
In vinyl fluoride reaction kettle, when insulation reaction 1-2 is small at 90-100 DEG C, discharge, dehydration, air drying obtains esterification kaolin；
（5）The stannous octoate mixing of above-mentioned esterification kaolin, 0.2-0.4 parts by weight is taken, is added in above-mentioned wax micro mist dispersion liquid,
It stirs evenly, kaolin micro mist dispersion liquid must be esterified；
（6）The formamide mixing of the SIS thermoplastic elastomer (TPE)s, 2-3 parts by weight of 27-30 parts by weight is taken, is added to mixture weight
In 1.6-2 times of absolute ethyl alcohol, when insulated and stirred 1-2 is small at 60-65 DEG C, ethyl alcohol is distilled off, obtains amination elastomer；
（7）Above-mentioned esterification kaolin micro mist dispersion liquid, the mixing of amination elastomer are taken, is stirred evenly, dropwise addition 18-20 parts by weight,
Concentration is the formalin of 10-14%, and rise temperature is 60-70 DEG C, and insulated and stirred 100-110 minutes is cooled to room temperature, obtains first
Base kaolin elastomer solution；
（8）Take the above-mentioned kaolin elastomer solution that methylates, the natural rubber, 4-5 parts by weight with 200-300 parts by weight it is anti-old
Agent rd is mixed, and is sent into mixer, mixing 30-40s, and mixing temperature is 60-100 DEG C, adds in the chlorination stone of 20-34 parts by weight
Wax is kneaded 6-8 minutes, dumping, is cooled to 20-30 DEG C, is put into open mill, adds in zinc oxide, the 2.8-3 of 0.7-1 parts by weight
The sulphur of parts by weight, the captax BS, thin logical 3-5 of 3-4 parts by weight are all over to get the insulating rubber material that methylates.
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| CN201710384695.1A CN107141524B (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method for the insulating rubber material that methylates |
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| CN201710384695.1A CN107141524B (en) | 2017-05-26 | 2017-05-26 | A kind of preparation method for the insulating rubber material that methylates |
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| CN107141524B true CN107141524B (en) | 2018-05-29 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381488A (en) * | 2008-11-04 | 2009-03-11 | 中国矿业大学(北京) | Kaolin/rubber nano compound material with strengthening and obstructing dual property |
| CN103555005A (en) * | 2013-10-12 | 2014-02-05 | 河曲县正阳高岭土有限公司 | Preparation method of modified kaolin used as rubber reinforcing agent |
| CN105461984A (en) * | 2015-12-17 | 2016-04-06 | 合肥杰明新材料科技有限公司 | Natural rubber material and preparing method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4790167B2 (en) * | 2001-07-27 | 2011-10-12 | 株式会社ブリヂストン | Natural rubber composition for tires |
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2017
- 2017-05-26 CN CN201710384695.1A patent/CN107141524B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381488A (en) * | 2008-11-04 | 2009-03-11 | 中国矿业大学(北京) | Kaolin/rubber nano compound material with strengthening and obstructing dual property |
| CN103555005A (en) * | 2013-10-12 | 2014-02-05 | 河曲县正阳高岭土有限公司 | Preparation method of modified kaolin used as rubber reinforcing agent |
| CN105461984A (en) * | 2015-12-17 | 2016-04-06 | 合肥杰明新材料科技有限公司 | Natural rubber material and preparing method thereof |
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