CN102643552B - Black flame-retardant silicon rubber material and preparation method thereof - Google Patents
Black flame-retardant silicon rubber material and preparation method thereof Download PDFInfo
- Publication number
- CN102643552B CN102643552B CN 201210156860 CN201210156860A CN102643552B CN 102643552 B CN102643552 B CN 102643552B CN 201210156860 CN201210156860 CN 201210156860 CN 201210156860 A CN201210156860 A CN 201210156860A CN 102643552 B CN102643552 B CN 102643552B
- Authority
- CN
- China
- Prior art keywords
- retardant
- preparation
- flame
- component
- black flame
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a black flame-retardant silicon rubber material and a preparation method thereof. The silicon rubber material is prepared by mixing and curing the following components in parts by mass: 50-60 parts of component A, 5-10 parts of component B, 0.1-0.3 part of catalyst and 29.7-44.9 parts of flame retardant. The component A is unvulcanized silicon rubber containing vinyl or propenyl terminal group; the component B is hydrogen-containing polysiloxane; the catalyst is a soluble platinic compound; and the flame retardant is a carbonized residue-diammonium hydrogen phosphate mixture obtained by pyrolyzing scrap tires. The carbonized residue-diammonium hydrogen phosphate mixture obtained by pyrolyzing scrap tires is used as the flame retardant to generate a synergic flame-retardant effect, thereby achieving the goal of preparation of the excellent-performace black flame-retardant silicon rubber material from the environment-friendly flame retardant, and more importantly, reutilizing the scrap tire resources; and thus, the invention has an important meaning for environmental protection business.
Description
Technical field
The present invention relates to a kind of black flame-retardant silastic material and preparation method thereof, specifically, relate to a kind of black flame-retardant silastic material that damaged tire makes and preparation method thereof that utilizes, belong to the material technology field.
Background technology
Along with the develop rapidly of transportation and automobile industry, tire production amount and rubber demand increase day by day, and the generation speed of junked tire is also sharply accelerated thereupon.Waste tire is difficult to decompose under field conditions (factors), and a large amount of accumulations can bring series of problems, for example: need a large amount of stockyards; Easily spontaneous combustion and be difficult to extinguish under the natural condition; Easily forming mosquito grows and brings pandemic etc. to cause the secondary public hazards.It is reported that 2010, China's tire production amount will reach more than 300,000,000, the generation of waste tire will reach more than 200,000,000 (heavily about 5,200,000 tons).How effectively to dispose quantity huge " black rubbish ", turn waste into wealth, deepen it and utilize degree, constructing economical society has become a difficult problem of needing solution badly.
The junked tire sustainable use mainly contains two large approach: the one, and old tire renovation; The 2nd, the damaged tire resource circulation utilization comprises and produces rubber powder, reclaimed rubber etc.It is carbon black filler that 35-40% is arranged in the damaged tire thermo-cracking approximately, but because ash content is very high, can only reach at most the performance level of soft carbon, is only applicable to some low grade products purposes.Because market is limited, and added value is very low, becomes a large bottleneck of thermo-cracking development.At present, report (Xue Yanli is arranged, junked tire has had new purposes, Chinese building material, 2004, (8)) claim that can adopt junked tire, waste plastic film is main raw material, add special auxiliary agent and catalyzed reaction agent, make a kind of Novel rubber plastic blend waterproof roll through the technical finesse of high-temperature blending Technology of Dynamic Vulcanized.Also can adopt junked tire to be processed in the compound that rubber powder is applied to bituminous pavement, not only can consume a part of junked tire, and can play certain Noise Reduction to bituminous pavement, has obvious economic benefit and social benefit (Meng Xiang horse, the application of junked tire in the road surface, the traffic stdn, 2010, (8)).(the Yan Dahai etc. such as Yan Dahai, XPS analysis of surface component of carbon blacks from pyrolysis of used tires in pilot-scale rotary kiln, the chemistry of fuel journal, 2005,33 (4)) rotary kiln pyrogenation damaged tire product pyrolysis oil and pyrolytic carbon characteristic have systematically been studied, investigated the situation of temperature to products collection efficiency and products distribution, measured pyrolytic carbon the gap structure characteristic and to its activation, in the hope of becoming the absorption macromole gac with business potential.Forever (forever honor of sun etc. such as flourish grade of sun, waste tyre pyrolytic reclaims the surface property research of carbon black, ACTA Scientiae Circumstantiae, 2002,22 (5)) by method modification waste tyre pyrolytic charcoals such as nitric acid acidwashing and stearic acid-nitric acid acidwashings, in the hope of structure and its surface property of raising that improves pyrolytic carbon.(the Wang Jinzhong etc. such as Wang Jinzhong, the waste tire fragment is done the embankment light filler, geotechnical engineering circle, 2005,9 (1)) then reported tire debris as the embankment light filler, because of its light weight, durable, good springiness, good water permeability, can improve surface deformation and drainage condition, be conducive to the stable of roadbed, have obvious technology, economy and environment benefit, the effective means that solves the waste tire environmental pollution of can yet be regarded as.
In sum as seen: at present be only limited to old tire renovation about the utilization of damaged tire and as light filler as material of construction, and utilize damaged tire to prepare the technology of black flame-retardant silastic material so far there are no relevant report.
Summary of the invention
For the existing defects of prior art and problem, the purpose of this invention is to provide a kind of black flame-retardant silastic material that damaged tire makes and preparation method thereof that utilizes, to realize the recycling purpose of damaged tire resource, promote the development of energy-conserving and environment-protective cause.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of black flame-retardant silastic material is got through mixing, solidifying by following component:
Described first component is the raw-silastic continuously that contains vinyl or propenyl end group; Described second component is hydrogen containing siloxane; Described catalyzer is the solubility platinic compound, that is, and and the platinic compound in soluble in water, sour, ethanol or the ether; The described fire retardant carbonization residue that to be damaged tire obtain through Pintsch process and the mixture of diammonium hydrogen phosphate.
As a kind of preferred version, described fire retardant is the mixture that is formed at 1: 3 in mass ratio by carbonization residue and diammonium hydrogen phosphate.
As a kind of preferred version, described carbonization residue is that the mixture by damaged tire and amino dodecane gets 400 ~ 600 ℃ of roastings.
A kind of preparation method of black flame-retardant silastic material of the present invention comprises the steps:
A) diammonium hydrogen phosphate, carbonization residue are added in the first component, stirring makes and mixes;
B) add second component and catalyzer, stirring makes and mixes;
C) to step b) mixture that obtains carries out ball milling;
D) material behind the ball milling is carried out vacuum exhaust, then be cured reaction at 20～40 ℃.
As a kind of preferred version, the preparation of described carbonization residue comprises the steps:
1. damaged tire is cut into sheet, then mixes in proportion with amino dodecane;
2. with said mixture 400 ~ 600 ℃ of roastings 4～6 hours;
3. cooling is pulverized, and crosses 200 ~ 300 mesh sieves.
As further preferred version, described damaged tire is 4: 1 ~ 9: 1 with the mixing quality ratio of amino dodecane.
As a kind of preferred version, step b) in catalyzer be Platinic chloride.
As a kind of preferred version, step c) in Ball-milling Time be 0.5～1.5 hour.
As a kind of preferred version, steps d) in vacuum exhaust refer to that in vacuum tightness be vacuum suction under 90～100Pa, the room temperature, discharge the bubble in the material.
As a kind of preferred version, steps d) in the curing reaction time be 24～48 hours.
Compared with prior art, the present invention has following unusual effect:
The present invention utilizes the mixture of carbonization residue that damaged tire obtains through Pintsch process and diammonium hydrogen phosphate as fire retardant, produced the cooperative flame retardant effect, make limiting oxygen index(LOI) and reached 32～35%, the thermal weight loss core temperature reaches 450～520 ℃, the black flame-retardant silastic material of mechanical property excellence, not only realized using the purpose of the black flame-retardant silastic material of environment amenable fire retardant processability excellence, the more important thing is, realized the recycling of damaged tire resource, for the recycling of damaged tire provides a new way, significant to the development of energy-conserving and environment-protective cause; And preparation method of the present invention is simple, is easy to realize industrialization, has practical value.
Embodiment
Following embodiment is by GB/T 1701-2001 and " nano composite polymer/laminated silicate material theory and practice " (QiZongNeng, Shang Wenyu writes, Chemical Industry Press, 2002) thermogravimetry of regulation carries out the test of mechanical property and the thermal weight loss core temperature of described silastic material; And according to GB 10707-89 regulation described silastic material is carried out the test of limiting oxygen index(LOI).
First component among the following embodiment is the raw-silastic continuously that contains vinyl ends, and is commercially available, and the trade mark of producing such as blue star organosilicon (Shanghai) Co., Ltd. is the A component product of RTV3040.
Second component among the following embodiment is hydrogen containing siloxane, and is commercially available, and the trade mark of producing such as blue star organosilicon (Shanghai) Co., Ltd. is the B component product of RTV3040.
Catalyzer among the following embodiment is the solubility platinic compound of soluble in water, sour, ethanol or ether, as: Platinic chloride.
The present invention is described in further detail and completely below in conjunction with embodiment.
Embodiment 1
80 gram waste tires are cut into sheet, and mix with 20 gram amino dodecanes; With the mixture crucible of packing into, put into retort furnace, in 400 ℃ of roastings 6 hours; Stopped heating, airtight cooling is taken out after the cooling, pulverizes 200 mesh sieves, gets the powdery carbonization residue.
33.7 gram diammonium hydrogen phosphates, the above-mentioned powdery carbonization residue of 11.2 grams are added in the 50 gram first components, and stirring at room 40 minutes mixes fire retardant and first component; Add 5 gram second components and 0.1 gram catalyzer, stirring at room 20 minutes mixes itself and fire retardant, first component again; Pour in the ball grinder of ball mill the mixture that obtains into room-temperature ball-milling 0.5 hour; Taking out, pour in the mould, is vacuum suction under 90Pa, the room temperature in vacuum tightness, to discharge bubble wherein; Be cured reaction 48 hours at 20 ℃; Take out, namely get black flame-retardant silastic material of the present invention.
Test result to mechanical property, thermal stability and the limiting oxygen index(LOI) of the black flame-retardant silastic material that obtains is shown in Table 1.
Comparative Examples 1
This Comparative Examples only is with the difference of embodiment 1: fire retardant is replaced with " 44.9 gram diammonium hydrogen phosphate " by " 33.7 gram diammonium hydrogen phosphates, the above-mentioned powdery carbonization residue of 11.2 grams "; All the other contents are all with identical described in the embodiment 1.
The color of the flame-proof silicon rubber material that this Comparative Examples obtains is white rather than black.
The test result of mechanical property, thermal stability and the limiting oxygen index(LOI) of the flame-proof silicon rubber material that this Comparative Examples is obtained is shown in Table 1.
Embodiment 2
85 gram waste tires are cut into sheet, and mix with 15 gram amino dodecanes; With the mixture crucible of packing into, put into retort furnace, in 500 ℃ of roastings 5 hours; Stopped heating, airtight cooling is taken out after the cooling, pulverizes 250 mesh sieves, gets the powdery carbonization residue.
27.6 gram diammonium hydrogen phosphates, the above-mentioned powdery carbonization residue of 9.2 grams are added in the 55 gram first components, and stirring at room 50 minutes mixes fire retardant and first component; Add 8 gram second components and 0.2 gram catalyzer, stirring at room 25 minutes mixes itself and fire retardant, first component again; Pour in the ball grinder of ball mill the mixture that obtains into room-temperature ball-milling 1 hour; Taking out, pour in the mould, is vacuum suction under 95Pa, the room temperature in vacuum tightness, to discharge bubble wherein; Be cured reaction 36 hours at 30 ℃; Take out, namely get black flame-retardant silastic material of the present invention.
Test result to mechanical property, thermal stability and the limiting oxygen index(LOI) of the black flame-retardant silastic material that obtains is shown in Table 1.
Comparative Examples 2
This Comparative Examples only is with the difference of embodiment 2: fire retardant is replaced with " 36.8 gram diammonium hydrogen phosphate " by " 27.6 gram diammonium hydrogen phosphates, the above-mentioned powdery carbonization residue of 9.2 grams "; All the other contents are all with identical described in the embodiment 2.
The color of the flame-proof silicon rubber material that this Comparative Examples obtains is white rather than black.
The test result of mechanical property, thermal stability and the limiting oxygen index(LOI) of the flame-proof silicon rubber material that this Comparative Examples is obtained is shown in Table 1.
Embodiment 3
90 gram waste tires are cut into sheet, and mix with 10 gram amino dodecanes; With the mixture crucible of packing into, put into retort furnace, in 600 ℃ of roastings 4 hours; Stopped heating, airtight cooling is taken out after the cooling, pulverizes 300 mesh sieves, gets the powdery carbonization residue.
22.3 gram diammonium hydrogen phosphates, the above-mentioned powdery carbonization residue of 7.4 grams are added in the 60 gram first components, and stirring at room 60 minutes mixes fire retardant and first component; Add 10 gram second components and 0.3 gram catalyzer, stirring at room 30 minutes mixes itself and fire retardant, first component again; Pour in the ball grinder of ball mill the mixture that obtains into room-temperature ball-milling 1.5 hours; Taking out, pour in the mould, is vacuum suction under 100Pa, the room temperature in vacuum tightness, to discharge bubble wherein; Be cured reaction 24 hours at 40 ℃; Take out, namely get black flame-retardant silastic material of the present invention.
Test result to mechanical property, thermal stability and the limiting oxygen index(LOI) of the black flame-retardant silastic material that obtains is shown in Table 1.
Comparative Examples 3
This Comparative Examples only is with the difference of embodiment 3: fire retardant is replaced with " 29.7 gram diammonium hydrogen phosphate " by " 22.3 gram diammonium hydrogen phosphates, the above-mentioned powdery carbonization residue of 7.4 grams "; All the other contents are all with identical described in the embodiment 3.
The color of the flame-proof silicon rubber material that this Comparative Examples obtains is white rather than black.
The test result of mechanical property, thermal stability and the limiting oxygen index(LOI) of the flame-proof silicon rubber material that this Comparative Examples is obtained is shown in Table 1.
The mechanical property of table 1 flame-proof silicon rubber material, thermal stability and limiting oxygen index(LOI) test result
By as seen from Table 1: the present invention utilizes the mixture of carbonization residue that damaged tire obtains through Pintsch process and diammonium hydrogen phosphate as fire retardant, produced the cooperative flame retardant effect, made that limiting oxygen index(LOI) reaches 32～35%, the thermal weight loss core temperature reaches 450～520 ℃, the black flame-retardant silastic material of mechanical property excellence.
In sum as seen: in the technology of the present invention, the carbonization residue that is obtained through Pintsch process by damaged tire that utilizes not only can play the tinting material effect, and have fire-retardant synergy; The present invention has not only realized using the purpose of the black flame-retardant silastic material of environment amenable fire retardant processability excellence, the more important thing is, realized the recycling of damaged tire resource, for the recycling of damaged tire provides a new way, significant to the development of energy-conserving and environment-protective cause; And preparation method of the present invention is simple, is easy to realize industrialization, has practical value.
Be necessary at last in this explanation to be, above embodiment is unrestricted the present invention in order to technical scheme of the present invention to be described only, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not breaking away from the spirit and scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (9)
1. a black flame-retardant silastic material is characterized in that, is got through mixing, solidifying by following component:
Described first component is the raw-silastic continuously that contains vinyl or propenyl end group; Described second component is hydrogen containing siloxane; Described catalyzer is the solubility platinic compound; The described fire retardant carbonization residue that to be damaged tire obtain through Pintsch process and the mixture of Secondary ammonium phosphate; Described carbonization residue is that the mixture by damaged tire and amino dodecane gets 400～600 ℃ of roastings.
2. black flame-retardant silastic material according to claim 1 is characterized in that: described fire retardant is by carbonization residue and the Secondary ammonium phosphate mixture that forms of 1:3 in mass ratio.
3. the preparation method of a black flame-retardant silastic material claimed in claim 1 is characterized in that, comprises the steps:
A) Secondary ammonium phosphate, carbonization residue are added in the first component, stirring makes and mixes;
B) add second component and catalyzer, stirring makes and mixes;
C) to step b) mixture that obtains carries out ball milling;
D) material behind the ball milling is carried out vacuum exhaust, then be cured reaction at 20～40 ℃.
4. the preparation method of black flame-retardant silastic material according to claim 3 is characterized in that, the preparation of described carbonization residue comprises the steps:
1. damaged tire is cut into sheet, then mixes in proportion with amino dodecane;
2. with said mixture 400～600 ℃ of roastings 4～6 hours;
3. cooling is pulverized, and crosses 200～300 mesh sieves.
5. the preparation method of black flame-retardant silastic material according to claim 4 is characterized in that: the mixing quality of described damaged tire and amino dodecane is than being 4:1～9:1.
6. the preparation method of black flame-retardant silastic material according to claim 3, it is characterized in that: the catalyzer step b) is Platinic chloride.
7. the preparation method of black flame-retardant silastic material according to claim 3, it is characterized in that: the Ball-milling Time step c) is 0.5～1.5 hour.
8. the preparation method of black flame-retardant silastic material according to claim 3, it is characterized in that: the vacuum exhaust steps d) refers to that in vacuum tightness be vacuum suction under 90～100Pa, the room temperature, discharges the bubble in the material.
9. the preparation method of black flame-retardant silastic material according to claim 3, it is characterized in that: the curing reaction time steps d) is 24～48 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210156860 CN102643552B (en) | 2012-05-17 | 2012-05-17 | Black flame-retardant silicon rubber material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210156860 CN102643552B (en) | 2012-05-17 | 2012-05-17 | Black flame-retardant silicon rubber material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102643552A CN102643552A (en) | 2012-08-22 |
| CN102643552B true CN102643552B (en) | 2013-10-30 |
Family
ID=46656641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210156860 Expired - Fee Related CN102643552B (en) | 2012-05-17 | 2012-05-17 | Black flame-retardant silicon rubber material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102643552B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106118065B (en) * | 2016-06-23 | 2019-04-30 | 上海工程技术大学 | A kind of expandable flame retardant silicon rubber and preparation method thereof |
| CN106753440B (en) * | 2016-12-29 | 2018-11-06 | 武汉工程大学 | The black paste generated in vitamin B6 industrial processes is in wood powder carbonization process as the application of fire retardant |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1285673C (en) * | 2004-12-22 | 2006-11-22 | 华南理工大学 | Fire-retardant silicon rubber and its preparation method |
| CN102134399B (en) * | 2011-05-06 | 2012-07-04 | 北京化工大学 | Flaming retarding highly conductive silicon rubber composite material and preparation method thereof |
-
2012
- 2012-05-17 CN CN 201210156860 patent/CN102643552B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102643552A (en) | 2012-08-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102977621A (en) | SBS (styrene-butadiene-styrene)/scrap rubber powder composite modified asphalt and preparation method thereof | |
| CN113636786B (en) | Emulsified asphalt plant-mixed cold recycled asphalt mixture and preparation method thereof | |
| CN101649122B (en) | SBS modified asphalt and preparation method thereof | |
| CN110981349A (en) | Light high-strength muck-based thermal insulation material and preparation method thereof | |
| CN102653631A (en) | Mixed asphalt for pavements and preparation method for mixed asphalt | |
| CN103435843A (en) | Reclaiming agent, reclaimed rubber prepared therefrom, and preparation method of reclaimed rubber | |
| CN102276024B (en) | Preparation method of structured micro-electrolysis packing used for treating wastewater, and structured micro-electrolysis packing | |
| CN102643552B (en) | Black flame-retardant silicon rubber material and preparation method thereof | |
| CN105384399A (en) | Method for preparing building materials by virtue of sludge pyrolyzation | |
| CN112159550A (en) | Method for preparing rubber by taking modified oil shale semi-coke as filler | |
| CN104987738A (en) | Waste rubber modified asphalt | |
| CN108163844B (en) | Preparation method for preparing graphene by using waste tire rubber powder | |
| CN112143039B (en) | Direct-vat M resin-based modified asphalt stabilizer, and preparation method and application thereof | |
| CN107118444A (en) | A kind of shoddy and PP intermingling materials and preparation method thereof | |
| CN105199669A (en) | Method for recycling waste carbon ceramic friction plate to prepare ceramic friction material | |
| CN102863187A (en) | Preparation method of used plastic regenerated plate | |
| CN102757198A (en) | Environment-friendly flaming retarding bituminous mixture and preparation method thereof | |
| CN110615928B (en) | Modified coal gangue powder filled polyolefin flame-retardant composite material and preparation process thereof | |
| CN115466099B (en) | Method for preparing water permeable brick by utilizing waste wind power blade | |
| CN109486234A (en) | A kind of waste plastic regeneration direct putting type asphalt mixed material modifier and preparation method thereof | |
| LU501453B1 (en) | The invention relates to a nanometer material composite waste rubber powder modified asphalt for heavy traffic roads and a preparation process thereof | |
| CN114507450B (en) | High-viscosity rubber modified asphalt and preparation method thereof | |
| CN104293150A (en) | Component B of polyurethane waterproof paint, preparation method of component B and polyurethane waterproof paint containing component B | |
| CN106278291B (en) | A kind of charging hole lid of coke oven sealing material and preparation method thereof | |
| CN104403331A (en) | Waterproof coiled material and method for preparing waterproof coiled material by using coal liquefaction residues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131030 |