CN106032434A - Powder rubber and vulcanized powder rubber, and preparation methods of powder rubber and vulcanized powder rubber - Google Patents
Powder rubber and vulcanized powder rubber, and preparation methods of powder rubber and vulcanized powder rubber Download PDFInfo
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Abstract
The present invention discloses a powder rubber and a preparation method thereof, and a vulcanized powder rubber and a preparation method thereof. The powder rubber comprises, by weight, 100 parts of a base rubber and 10-150 parts of a flame retardant. The vulcanized powder rubber is prepared by vulcanizing the powder rubber, wherein the vulcanization conditions are that the vulcanization temperature is 120-170 DEG C and the vulcanization time is 10-50 min. According to the present invention, the prepared powder rubber and the prepared vulcanized powder rubber have characteristics of small particle size, uniform distribution, fire retardation property, and toughening property, and the preparation method is simple.
Description
Technical field
The present invention relates to powdered rubber and sulfide powder rubber and preparation method thereof and by described method system
The powdered rubber obtained and sulfide powder rubber.
Background technology
Along with developing rapidly of science and technology, plastics, rubber and fiber have become widely used high score
Sub-material, but macromolecular material is the most inflammable.2010-2013, dead 386 people of China's fire are injured
1967 people, cause direct property loss 5,200,000,000 yuan, and the indirect economic loss caused is bigger, and causes this
One of a little leading cause of fires are exactly that macromolecular material is inflammable.Therefore, improve macromolecular material and
The fire resistance of product is significant.
The carbon bond rubber polymer containing halogen, when being heated to uniform temperature, first decomposes dehydrohalogenation
(HF, HCl), also can decomposite flammable Hydrocarbon, but hydrogen halides is incombustibility material,
Serve the fire retardation isolated oxygen, water down the concentration of inflammable substance.The most this material difficulty is fired
There is self-extinguishment, be intrinsic fire proofing, such as fluorubber, neoprene, chlorosulfonated polyethylene and chlorine
Change polyethylene etc..
Silicone rubber is polymer based on hydroxyl-terminated injecting two methyl siloxane, the silica chain in its strand
Can promote that material at high temperature becomes charcoal during joint burning, contribute to forming antioxidative protective layer, have one
Determine fire retardation, and volume of smoke and harmful gas will not be produced.
Powdered rubber has to be easy to measure, be beneficial to realize process automation and serialization, shortening mixing time
With extend the advantage such as time of scorch, deeply paid attention to by rubber industry field.20 th century later, powder rubber
Glue is widely used in rubber, binding agent and polymer modification field, defines with block glue (raw
Blob of viscose and vulcanizing agent), latex, glue and suspension be base material, to become powder technology and isolation technology as base
The multiple preparation method of plinth, wherein spray drying method is the main method that latex becomes powder with glue, preparation
The powdered rubber granule gone out is tiny, rounding.CN1330097A discloses a kind of fully sulfurized silicon rubber powder
And preparation method thereof, the method chooses low-molecular-weight organosilicon polymer or copolymer emulsion is raw material,
By cross-linking radiation, rubber particles particle diameter is fixed, be then dried by spray drying method,
To the fully sulfurized silicon rubber powder of particle diameter≤1 μm, but, this silicon rubber powder only possesses toughening effect,
There is no good fire resistance.
As can be seen here, need to select suitable glue kind to prepare powdered rubber so that it is be provided simultaneously with fire-retardant with
Toughness reinforcing performance.
Summary of the invention
The invention aims to overcome the defect that the fire resistance of existing powdered rubber material is poor,
Provide a kind of powdered rubber and preparation method thereof.
The present inventor is found by further investigation, by adding in the preparation process of powdered rubber
Adding fire retardant, the powdered rubber being possible not only to make to prepare has fire resistance, and fire-retardant by controlling
The consumption of agent, it is possible to obtain the powder of preferable particle size range (such as mean diameter 100-200 nanometer)
Rubber.Its principle is speculated as: in organic solvent, scattered fire retardant plays hard template effect, will be by basis
The latex particle that rubber solution is formed separates, and obtains different particle diameter distributions, is then the most additionally adding
With using spray drying method in the case of interleaving agent, obtain the particle diameter powdered rubber less than 200nm.
The invention provides a kind of powdered rubber, described powdered rubber contains base rubber and fire retardant,
Relative to the base rubber of 100 weight portions, the content of fire retardant is 10-150 weight portion.
Invention further provides the preparation method of a kind of powdered rubber, it is characterised in that the method bag
Include: under conditions of stirring, base rubber is dissolved in organic solvent and contacts with fire retardant, so
After mixture that contact is obtained be spray-dried.
Present invention also offers the powdered rubber prepared by said method, the particle diameter of this powdered rubber is
50-700nm, preferably 100-200nm.
Present invention also offers a kind of sulfide powder rubber, this sulfide powder rubber is provided by the present invention
Powdered rubber sulfuration prepares, and the condition of described sulfuration includes: the temperature of sulfuration is 120-170 DEG C, sulfuration
Time be 10-50 minute.
The advantage of the powdered rubber of present invention offer and sulfide powder rubber and preparation method thereof is embodied in:
1) present invention offer and the powdered rubber of preparation and sulfide powder rubber have fire-retardant and toughness reinforcing simultaneously
Performance；
2) present invention provide and the powdered rubber of preparation and sulfide powder rubber size little and be evenly distributed；
3) preparation technology of the present invention is simple；
4) present invention provide and preparation powdered rubber and the nontoxic Halogen of sulfide powder rubber, for environmental protection hinder
Combustion toughener.
Other features and advantages of the present invention will give specifically in detailed description of the invention part subsequently
Bright.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place
The detailed description of the invention described is merely to illustrate and explains the present invention, is not limited to the present invention.
First aspect present invention provides a kind of powdered rubber, described powdered rubber contain base rubber and
Fire retardant.From the angle that can either realize enough fire resistances and be obtained in that again required particle diameter,
Relative to the base rubber of 100 weight portions, the content of fire retardant can be 10-150 weight portion, preferably
Ground, relative to the base rubber of 100 weight portions, the content of fire retardant is 20-100 weight portion.This
Bright inventor finds in an experiment, relative to the base rubber of 100 weight portions, when the content of fire retardant
During for 10-150 weight portion, the particle diameter of prepared powdered rubber is usually 50-700nm；Relative to 100
The base rubber of weight portion, when the content of fire retardant is 20-100 weight portion, prepared powdered rubber
Particle diameter be usually 100-200nm.
Powdered rubber described according to a first aspect of the present invention, the particle diameter of this powdered rubber can be
50-700nm, preferably 100-200nm.In the present invention, the particle diameter of powdered rubber is moved by laser
State light scattering or projection Electronic Speculum detection.
Powdered rubber described according to a first aspect of the present invention, described base rubber can be that this area is normal
The base rubber for preparing powdered rubber of rule, is preferably self basic rubber with fire resistance
One or more in glue, more preferably silicone rubber, fluorubber and halogenated butyl rubber, the most excellent
Elect silicone rubber as.Preferably, described silicone rubber be dimethyl silicone rubber, methyl vinyl silicone rubber,
Methyl vinyl phenyl silicone rubber, methyl ethylene trifluoro propyl silicone rubber, phenylene silicone rubber, phenylate
One or more in support silicone rubber, nitrile silicone rubber and silicon boron rubber, more preferably methyl ethylene silicon rubber
Glue.Preferably, described halogenated butyl rubber is neoprene.
Powdered rubber described according to a first aspect of the present invention, described fire retardant can be that halogen system is fire-retardant
Agent, nitrogenated flame retardant, phosphorus-nitrogenated flame retardant, Sb system fire retardant, Phos flame retardant, halogen-phosphorus system
One in fire retardant, aluminum-magnesium series fire retardant, silicon-series five-retardant, boron flame retardant and molybdenum flame retardant
Or multiple, preferably Al (OH)3And/or Mg (OH)2.The present inventor sends out in process of the test
Existing, choose Al (OH)3And/or Mg (OH)2Less the dividing with particle diameter of particle diameter can be obtained as fire retardant
Cloth powdered rubber evenly, its principle is speculated as: in solvent, the hydroxyl on scattered fire retardant surface leads to
Cross the water-wet side with micellar surface and form intermolecular hydrogen bonding, scattered monomer in the continuous lyosoption of micelle
Drop and form latex particle, the now hard template effect of fire retardant limits the size of latex particle,
And then again by controlling the consumption of fire retardant, increase fire retardant several with the combination of the water-wet side of micellar surface
Rate so that latex particle presents certain particle diameter distribution.
Powdered rubber described according to a first aspect of the present invention, described powdered rubber possibly together with vulcanizing agent,
Being in terms of 100 weight portions by base rubber content, the content of vulcanizing agent is 1-3 weight portion.Described vulcanizing agent
Can be organic peroxide, it is preferable that described vulcanizing agent be benzoyl peroxide, 2,4-dichloro peroxide
Change benzoyl, t-butyl perbenzoate, di-t-butyl peroxide, cumyl peroxide and 2,5-diformazan
Base-2, one or more in 5-di-t-butyl hexane peroxide, it is further preferred that described vulcanizing agent
For cumyl peroxide.
Second aspect present invention provides the preparation method of a kind of powdered rubber, it is characterised in that the party
Method includes: under conditions of stirring, is dissolved in organic solvent by base rubber and connects with fire retardant
Touching, the mixture then contact obtained is spray-dried.
Preparation method described according to a second aspect of the present invention, in order to realize the purpose of the present invention, relatively
In the base rubber of 100 weight portions, the consumption of fire retardant can be 10-150 weight portion, is preferably
20-100 weight portion.
Preparation method described according to a second aspect of the present invention, the consumption of described organic solvent is the most especially
Restriction, it is possible to base rubber is dissolved, it is preferable that relative to the base rubber of 1g, described
The consumption of organic solvent can be 10-100ml.Described dissolving refers to that base rubber can reach organic
And the state of solid phase that be visible by naked eyes mutually fully dispersed with flowing in solvent.
Preparation method described according to a second aspect of the present invention, the condition of described stirring the most particularly limits
Fixed, the purpose of the present invention can be realized, from the point of view of saving the energy, can at room temperature enter
OK.
Preparation method described according to a second aspect of the present invention, base rubber is dissolved in organic solvent
There is no particular limitation for mixing time, it is possible to is dissolved by base rubber, preferably 20-28 hour；
The time contacted with fire retardant by the base rubber being dissolved in organic solvent, also there is no particular limitation,
Can mix homogeneously, preferably 1-15 hour, more preferably 2-8 hour.
Preparation method described according to a second aspect of the present invention, described spray drying can use this area
Conventional spray drying device and condition, it is preferable that the inlet temperature of spray drying device can be controlled
For 100-180 DEG C, outlet temperature is 20-80 DEG C.
Preparation method described according to a second aspect of the present invention, described organic solvent can be that this area is normal
The organic solvent for preparing powdered rubber of rule, preferably the one of toluene, trichloro ethylene and butanone
Plant or multiple, more preferably toluene.
Preparation method described according to a second aspect of the present invention, in order to obtain the powdered rubber of smaller particle
And improve safety and drying efficiency when being spray-dried, can be dissolved at base rubber organic molten
After agent, before contacting with fire retardant, by the mixed liquor diluent of base rubber Yu organic solvent
Dilution, described diluent is preferably water.There is no particular limitation for the consumption of described water, it is preferable that institute
The volume ratio stating water and organic solvent is 0.5-10:1, more preferably 1-8:1.Described base rubber with
The time that the stirring of the mixed liquor of organic solvent and water contact is not particularly limited, it is possible to by base rubber and
The mixed liquor of organic solvent is mixed homogeneously with water, preferably 0.5-5 hour, and more preferably 1-3 is little
Time.
Preparation method described in second aspect present invention also includes: described contact is in the presence of vulcanizing agent
Carrying out, the consumption of described vulcanizing agent is the use of the vulcanizing agent of interpolation when preparing rubber that this area is conventional
Amount, it is preferable that relative to the base rubber of 100 weight portions, the consumption of vulcanizing agent is 1-3 weight portion.
Preparation method described according to a second aspect of the present invention, described vulcanizing agent is suitable with the addition of fire retardant
There is no particular limitation for sequence, can be simultaneously introduced, it is also possible to be sequentially added into, and the present inventor sends out
Now vulcanizing agent and fire retardant being sequentially added into and can obtain more preferable toughening effect, its principle is speculated as depending on
The secondary uniformity that there was added beneficially sulphide bond distribution.
Base rubber, fire retardant and vulcanizing agent described in second aspect present invention and first aspect present invention
Described base rubber, fire retardant are identical with vulcanizing agent, do not repeat them here.
Present invention also offers powdered rubber prepared by the most described method, this powder
The particle diameter of end rubber is 50-700nm, preferably 100-200nm.
Third aspect present invention provides a kind of sulfide powder rubber, and this sulfide powder rubber is by the present invention
The powdered rubber sulfuration provided prepares, and the condition of described sulfuration includes: the temperature of sulfuration is
120-170 DEG C, the time of sulfuration is 10-50 minute.
Sulfide powder rubber described according to a third aspect of the present invention, when containing sulfur in described powdered rubber
During agent, this powdered rubber is directly vulcanized prepared sulfide powder rubber；When in described powdered rubber not
During containing vulcanizing agent, first the described powdered rubber of the vulcanizing agent of 1-3 weight portion with about 100 weight portions is connect
Touching, then revulcanization prepares sulfide powder rubber.
Sulfide powder rubber described according to a third aspect of the present invention, the particle diameter of this sulfide powder rubber is
50-700nm, preferably 100-200nm.
The powdered rubber of the present invention and sulfide powder rubber can be carried out in the way of this area is conventional should
With, such as can use as the additive in process of producing product, preferably as Merlon, gather
The modifying agent of the polymer such as vinyl chloride (PVC), phenolic resin and epoxy resin, to increase polymer
Toughness also reduces combustibility.
The following examples will assist in the explanation present invention, but does not limit to its scope.
The particle diameter of powdered rubber is detected by dynamic laser light scattering experimental Electronic Speculum.
In the case of not having specified otherwise, reagent used in following example is both from being purchased.
Embodiment 1-4 is for illustrating powdered rubber that the present invention provides and sulfide powder rubber and preparation side thereof
Method.
Embodiment 1
Take the methyl vinyl phenyl silicone rubber (Shanghai Resin Factory Co., Ltd., the trade mark: 120) of 100g,
Being placed in a container, add 1L trichloro ethylene, stir 28 hours, add 8L water, stirring 2 is little
Time, then while stirring, it is sequentially added into 1g vulcanizing agent di-t-butyl peroxide and 150g fire retardant
Mg(OH)2, continue stirring and reach mix homogeneously in 2 hours, obtain polymer emulsion.By this polymer latex
Breast is spray-dried, and the inlet temperature controlling spray drying device is 100 DEG C, and outlet temperature is
20 DEG C, in cyclone separator, then collect the powdered rubber obtained after drying, gained powdered rubber
Mean diameter is about 450nm.
The powdered rubber obtained after being spray-dried is placed in the thermo-oxidative ageing case of temperature 120 DEG C sulfuration
20min, obtains sulfide powder rubber, and the mean diameter of gained sulfide powder rubber is about 450nm.
Embodiment 2
Take the dimethyl silicone rubber (Zhong Hao Chenguang Research Institute of Chemical Industry company limited, the trade mark: 101) of 100g,
Being placed in a container, add 4L butanone, stir 20 hours, add 12L water, stirring 2 is little
Time, then while stirring, it is sequentially added into 2g vulcanizing agent t-butyl perbenzoate and 100g fire retardant
Al(OH)3, continue stirring and reach mix homogeneously in 6 hours, obtain polymer emulsion.By this polymer latex
Breast is spray-dried, and the inlet temperature controlling spray drying device is 180 DEG C, and outlet temperature is
80 DEG C, in cyclone separator, then collect the silicon rubber powder obtained after drying, gained powdered rubber
Mean diameter be about 200nm.
The powdered rubber obtained after spray drying is placed in the thermo-oxidative ageing case of temperature 170 DEG C, sulfuration
40min, obtains sulfide powder rubber, and the mean diameter of gained sulfide powder rubber is about 200nm.
Embodiment 3
Take the methyl vinyl silicone rubber (Shanghai Resin Factory Co., Ltd., the trade mark: 120) of 100g, put
In a container, add 4L toluene, stir 24 hours, add 6L water, stir 3 hours, so
After stirring while, be sequentially added into 2g vulcanizing agent cumyl peroxide (DCP) and 80g fire-retardant
Agent Al (OH)3, continue stirring and reach mix homogeneously in 8 hours, obtain polymer emulsion.By this polymer
Latex is spray-dried, and the inlet temperature controlling spray drying device is 140 DEG C, and outlet temperature is
50 DEG C, in cyclone separator, then collect the silicon rubber powder obtained after drying, gained powdered rubber
Mean diameter be about 150nm.
Obtain being placed in the powdered rubber of gained in the thermo-oxidative ageing case of temperature 150 DEG C after being spray-dried,
Sulfuration 30min, obtains sulfide powder rubber, and the mean diameter of gained sulfide powder rubber is about
150nm。
Embodiment 4
Take the neoprene (NEC chemical industry Co., Ltd., the trade mark: PM40-NS) of 100g,
Being placed in a container, add 10L toluene, stir 18 hours, add 10L water, stirring 0.5 is little
Time, then while stirring, it is sequentially added into 3g vulcanizing agent DCP and 10g fire retardant Al (OH)3,
Continue stirring and reach mix homogeneously in 12 hours, obtain polymer emulsion.This polymer emulsion is sprayed
Mist is dried, and the inlet temperature controlling spray drying device is 190 DEG C, and outlet temperature is 90 DEG C, then exists
Collecting the silicon rubber powder obtained after drying in cyclone separator, the mean diameter of gained powdered rubber is
400nm。
The powdered rubber obtained after being spray-dried is placed in the thermo-oxidative ageing case of temperature 110 DEG C, sulfuration
50min, obtains sulfide powder rubber, and the mean diameter of gained sulfide powder rubber is about 400nm.
Comparative example 1
Powdered rubber and sulfide powder rubber is prepared according to the method described in the embodiment 1 of CN1330097A
Glue.The mean diameter of gained powdered rubber is about 200nm, and the mean diameter of gained sulfide powder rubber is about
For 200nm.
Powdered rubber prepared by embodiment 1-4 and comparative example 1 and sulfide powder rubber are used following side
Method tests its notch impact strength (J/m-1) and UL94 burning rank, wherein, notch impact strength
(J/m-1) and UL94 burning rank characterize toughness reinforcing performance and fire resistance respectively, the results are shown in Table 1 institute
Show.
Taking notch impact strength is 172.6J/m-1, UL94 burning rank be the Merlon of V-2, by powder
End rubber or sulfide powder rubber and this Merlon with the weight ratio at room temperature premixing of 40:100 it
Melt extruded by double screw extruder afterwards, pelletize；Extrusion temperature is 240-260 DEG C, and die temperature is
250 DEG C, screw speed is 200r/min.Injection machine injection mo(u)lding used after drying by extrusion pellet, obtains
Vertical combustion, nick break test standard testing batten, the notch shock then testing this composite is strong
Degree and UL94 burning rank, particularly as follows:
1) notch impact strength: according to standard ASTM D256, uses Mei Site Industrial Co., Ltd
ZBC1151 type shock machine carries out toughness reinforcing performance test, and notch impact strength is the biggest, illustrates compound
The toughness reinforcing performance of material is the best；
2) UL94 burning rank: according to standard ASTM D3801/UL94, uses CZF type level to hang down
Direct combustion burn the analyzer fire resistance test analysis to composite, the fire resistance of composite along with
Flame retardant rating V-0, V-1, V-2, HB are gradually deteriorated.
Table 1
Comparative example and comparative example are it can be seen that use powder rubber prepared by the method for present invention offer
Glue and sulfide powder rubber have more preferable toughness reinforcing performance and fire resistance.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned
Detail in embodiment, in the technology concept of the present invention, can be to the skill of the present invention
Art scheme carries out multiple simple variant, and these simple variant belong to protection scope of the present invention.
Claims (14)
1. a powdered rubber, described powdered rubber contains base rubber and fire retardant, relative to 100
The base rubber of weight portion, the content of fire retardant is 10-150 weight portion.
Powdered rubber the most according to claim 1, wherein, relative to the basis of 100 weight portions
Rubber, the content of fire retardant is 20-100 weight portion.
Powdered rubber the most according to claim 1 and 2, wherein, the particle diameter of described powdered rubber
For 50-700nm, preferably 100-200nm.
4. according to the powdered rubber described in any one in claim 1-3, wherein, described basis rubber
Glue is one or more in silicone rubber, fluorubber and halogenated butyl rubber, preferably silicone rubber.
5. according to the powdered rubber described in any one in claim 1-4, wherein, described fire retardant
For Al (OH)3And/or Mg (OH)2。
6. according to the powdered rubber described in any one in claim 1-5, wherein, described powder rubber
Glue, possibly together with vulcanizing agent, is in terms of 100 weight portions by base rubber content, and the content of vulcanizing agent is 1-3 weight
Amount part.
Powdered rubber the most according to claim 6, wherein, described vulcanizing agent is organic peroxy
Thing；Preferably, described vulcanizing agent be benzoyl peroxide, 2,4-dichlorobenzoperoxide, cross benzene first
Tert-butyl acrylate, di-t-butyl peroxide, cumyl peroxide and 2,5-dimethyl-2,5-di-t-butyl mistake
One or more in oxidation hexane, it is further preferred that described vulcanizing agent is peroxidating diisopropyl
Benzene.
8. the preparation method of a powdered rubber, it is characterised in that the method includes: at the bar of stirring
Under part, base rubber it is dissolved in organic solvent and contacts with fire retardant, then contact being obtained
Mixture is spray-dried.
Preparation method the most according to claim 8, wherein, relative to the basis of 100 weight portions
Rubber, the consumption of fire retardant is 10-150 weight portion, preferably 20-100 weight portion.
The most according to claim 8 or claim 9, preparation method, wherein, described organic solvent is first
One or more in benzene, trichloro ethylene and butanone, preferably toluene.
11. preparation methoies described in any one in-10 according to Claim 8, wherein, described contact
Carrying out in the presence of vulcanizing agent, relative to the base rubber of 100 weight portions, the consumption of vulcanizing agent is
1-3 weight portion.
12. powdered rubbers prepared by the method described in any one in claim 8-11, described powder
The particle diameter of end rubber is 50-700nm, preferably 100-200nm.
13. 1 kinds of sulfide powder rubber, this sulfide powder rubber is by any in claim 1-7 and 12
One described powdered rubber sulfuration prepares, and the condition of described sulfuration includes: the temperature of sulfuration is
120-170 DEG C, the time of sulfuration is 10-50 minute.
14. sulfide powder rubber according to claim 13, wherein, described sulfide powder rubber
Particle diameter be 50-700nm, preferably 100-200nm.
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| CN106832936A (en) * | 2016-12-30 | 2017-06-13 | 安徽凌宇电缆科技有限公司 | A kind of aging-resistant flame-proof cable cover(ing) formula |
| CN109467934A (en) * | 2018-10-29 | 2019-03-15 | 江苏宏鹏电气科技有限公司 | A kind of anti-aging cable insulation layer formula of high temperature resistant |
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| CN103159867A (en) * | 2011-12-15 | 2013-06-19 | 中国石油天然气股份有限公司 | Preparation method of flame-retardant powdered rubber |
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| JPH05230289A (en) * | 1992-02-19 | 1993-09-07 | Bridgestone Corp | Flame-retardant rubber composition |
| CN101182376A (en) * | 1998-12-18 | 2008-05-21 | Pku粉末橡胶联合有限公司 | Process for making compounded rubber powders |
| CN1402752A (en) * | 1999-12-03 | 2003-03-12 | 中国石油化工集团公司 | Full vulcanized powdered rubber with controllable particle diameter, preparing method thereof |
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| CN109467934A (en) * | 2018-10-29 | 2019-03-15 | 江苏宏鹏电气科技有限公司 | A kind of anti-aging cable insulation layer formula of high temperature resistant |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106032434B (en) | 2019-12-20 |
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