CN106751898A - A kind of Black flame-retardant silicon rubber material and preparation method thereof - Google Patents
A kind of Black flame-retardant silicon rubber material and preparation method thereof Download PDFInfo
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- CN106751898A CN106751898A CN201611136024.5A CN201611136024A CN106751898A CN 106751898 A CN106751898 A CN 106751898A CN 201611136024 A CN201611136024 A CN 201611136024A CN 106751898 A CN106751898 A CN 106751898A
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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
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of Black flame-retardant silicon rubber material, including following weight portion raw material：40~60 parts of rubber, 30~50 parts of reinforced filling, 1~3 part of nano titanium oxide, 2~5 parts of vulcanizing agent, 1~3 part of surfactant, 3~8 parts of adhesive, 2~5 parts of fire retardant.A kind of Black flame-retardant silicon rubber material proposed by the present invention, it has good anti-aging, oil resistant, it is heat-resisting, acid-alkali-corrosive-resisting performance, elasticity, good flame resistance, the present invention does reinforced filling using rubber powder prepared by waste tire, effectively raise the mechanical property of gained silicon rubber, while silicon rubber combination property is ensured, twice laid is accomplished, reduce the wasting of resources, it is effectively protected environment, its preparation method is simple to operate, preparation condition is gentle, preparation cost is low, gained black flame-retardant silicon rubber can be widely applied to electric wire, electronic apparatus, instrument, sealing ring, pad and other field.
Description
Technical field
The present invention relates to synthetic material technical field, more particularly to a kind of Black flame-retardant silicon rubber material and its preparation side
Method.
Background technology
Silicon rubber refers to that main chain is alternately made up of silicon and oxygen atom, and generally two rubbers of organic group are connected with silicon atom
Glue.Common silicon rubber is mainly made up of the silica chain link containing methyl and a small amount of vinyl.The introducing of phenyl can improve silicon rubber
High- and low-temperature resistance performance, the introducing of trifluoro propyl and cyano group can then improve the heatproof and oil resistance of silicon rubber.Silicon rubber is resistance to low
Temperature is functional, typically remains to work at -55 DEG C.After introducing phenyl, reachable -73 DEG C.The heat resistance of silicon rubber is also very prominent
Go out, at 180 DEG C can long-term work, a little higher than 200 DEG C can also bear several weeks or longer time it is still flexible, be instantaneously resistant to 300
High temperature more than DEG C.The good permeability of silicon rubber, OTR oxygen transmission rate is highest in synthetic polymer.High-temperature silicon disulfide rubber
Refer to the process of that polysiloxanes change elastomer-forming is by high temperature (110-170 DEG C) sulfidization molding.It is main with HMW
Polymethyl methacrylate be rubber, be mixed into reinforced filling, vulcanizing agent etc., heat pressurization under vulcanize elastomer-forming.Silicon
The reinforcement of rubber is mainly various types of white carbons, can make the intensity of vulcanizate and increase decades of times.
Tire is the annular elastic rubber product rolled in various vehicles or the ground connection mechanically assembled, and tire consumes rubber
Glue amount is huge, and the world consumes the half of rubber mass all for the production of tire, and over more than 60 years, China progressively develops founding of New
As the big producer of world's tire industry first.The Main Ingredients and Appearance of automobile tire material is natural rubber or synthetic rubber, naturally
The combination property of rubber is superior to cross synthetic rubber, the senior multiplex natural rubber of tire, in order that there is rubber manufacture tire to must
Must performance, in the production process of tire, it is necessary to add different auxiliary agents, wherein can substantial amounts of addition carbon black because carbon have
There is special adsorptivity, carbon particle is very good with the bonding of rubber molecule, effectively enhance rubber hardness, intensity and wear-resisting
Property, therefore, automobile tire main material is the composite of a kind of rubber and carbon black.With transportation and automobile industry
Develop rapidly, the output of tire is sharply increased, the generation speed of thing followed waste tire is also drastically increased.Due to discarded
Tire does not possess self-degradation, is difficult to decompose under field conditions (factors), result in the substantial amounts of accumulation of waste tire, big so as to bring
Amount occupied ground, easily grows germ, easily triggers a series of problems such as fire.Waste tire is processed into for a disaster
Topic.Based on above statement, the present invention proposes a kind of Black flame-retardant silicon rubber material and preparation method thereof.
The content of the invention
The invention aims to solve shortcoming present in prior art, and a kind of black flame-retardant silicon rubber for proposing
Material and preparation method thereof.
A kind of Black flame-retardant silicon rubber material, including following weight portion raw material：40~60 parts of rubber, reinforced filling 30~
50 parts, 1~3 part of nano titanium oxide, 2~5 parts of vulcanizing agent, 1~3 part of surfactant, 2~5 parts of structure inhibitor, adhesive
3~8 parts, 2~5 parts of fire retardant.
Preferably, a kind of raw material of described Black flame-retardant silicon rubber material, including following weight portion：Rubber 45~55
Part, 35~45 parts of reinforced filling, 1.5~2.5 parts of nano titanium oxide, 3~4 parts of vulcanizing agent, 1.5~2.5 parts of surfactant,
3~4 parts of structure inhibitor, 4~7 parts of adhesive, 3~4 parts of fire retardant.
Preferably, a kind of raw material of described Black flame-retardant silicon rubber material, including following weight portion：50 parts of rubber, benefit
Strong 40 parts of filler, 2 parts of nano titanium oxide, 3.5 parts of vulcanizing agent, 2 parts of surfactant, 3.5 parts of structure inhibitor, adhesive 5
Part, 3.5 parts of fire retardant.
Preferably, the rubber is the poly- methyl vinyl silicone rubber of HMW.
Preferably, the reinforced filling is recovery tire devulcanized rubber.
Preferably, the vulcanizing agent is perbenzoic acid, excessively sad tert-pentyl ester, tert-butyl peroctoate, MEK peroxide
One or more in compound, peroxide sulphonyl class and ketal peroxide class.
Preferably, described adhesive is liquid silastic.
The invention allows for a kind of preparation method of Black flame-retardant silicon rubber material, comprise the following steps：
S1, waste tire is broken into tire meal, is cleaned using 55~75 DEG C of running water, be then with concentration
68~85% ethanol water soaks 4~8h, is dried after centrifuge impurity elimination, must dry meal；
S2, in mass ratio 2~5:0.3~0.5, will dry after meal is mixed with coal tar and add regeneration reactor
In, after 18~24h of regeneration, obtain reinforced filling；
S3, the rubber of the proportion and reinforced filling add kneader, mixed at a high temperature of 120~200 DEG C
Refining, sequentially adds surfactant, nano titanium oxide, adhesive and fire retardant, the turning with 100~300r/min when adding
Speed is mixed, and 50~70 DEG C of insulations are cooled to after 6~10h of mixing, obtains blend glue stuff；
S4, the vulcanizing agent of the proportion is added in the compound being incubated in step S3, continue to stir mixing 25~
50min, using double screw extruder, the extruding pelletization at 128~145 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
A kind of Black flame-retardant silicon rubber material proposed by the present invention, it has good anti-aging, oil resistant, heat-resisting, acidproof
Caustic corrosion performance, elasticity, good flame resistance, the present invention does reinforced filling using rubber powder prepared by waste tire, effectively raises
The mechanical property of gained silicon rubber, while silicon rubber combination property is ensured, has accomplished twice laid, reduces resource wave
Take, be effectively protected environment, the invention allows for a kind of preparation method of Black flame-retardant silicon rubber material, to waste tire
Reinforced filling is prepared after reclaiming desulfurization process, black flame-retardant silicon rubber, this hair is obtained after being kneaded with rubber and addition auxiliary agent
The preparation method of bright proposition is simple to operate, preparation condition is gentle, does reinforced filling using waste tire and effectively reduces preparation
Cost, preparation cost is low, gained black flame-retardant silicon rubber can be widely applied to electric wire, electronic apparatus, instrument, sealing ring,
Pad and other field.
Specific embodiment
The present invention is made with reference to specific embodiment further explain.
Embodiment one
A kind of Black flame-retardant silicon rubber material proposed by the present invention, including following weight portion raw material：HMW it is poly-
45 parts of methyl vinyl silicone rubber, 40 parts of recovery tire devulcanized rubber, 2 parts of nano titanium oxide, excessively sad 4 parts of tert-pentyl ester, table
2 parts of face activating agent, structure inhibitors 4 part, 6 parts of liquid silastic, 4 parts of fire retardant.
Its preparation method, comprises the following steps：
S1, waste tire is broken into tire meal, is cleaned using 70 DEG C of running water, be then 80% with concentration
Ethanol water immersion 5h, after centrifuge impurity elimination dry, meal must be dried；
S2, in mass ratio 4:0.3, will dry after meal is mixed with coal tar in addition regeneration reactor, regeneration 20h
Afterwards, tire devulcanized rubber must be reclaimed；
S3, the poly- methyl vinyl silicone rubber of the HMW of the proportion and recovery tire devulcanized rubber are added and is mediated
In machine, kneaded at a high temperature of 180 DEG C, sequentially added surfactant, nano titanium oxide, liquid silastic and fire-retardant
Agent, is mixed when adding with the rotating speed of 200r/min, and 60 DEG C of insulations are cooled to after mixing 8h, obtains blend glue stuff；
S4, the excessively sad tert-pentyl ester of the proportion is added in the compound being incubated in step S3, continues to stir mixing
40min, using double screw extruder, the extruding pelletization at 130 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
Embodiment two
A kind of Black flame-retardant silicon rubber material proposed by the present invention, including following weight portion raw material：HMW it is poly-
50 parts of methyl vinyl silicone rubber, reclaim 35 parts of tire devulcanized rubber, 1.5 parts of nano titanium oxide, 2 parts of perbenzoic acid,
1 part of surfactant, 2 parts of structure inhibitor, 8 parts of liquid silastic, 2 parts of fire retardant.
Its preparation method, comprises the following steps：
S1, waste tire is broken into tire meal, is cleaned using 65 DEG C of running water, be then 68% with concentration
Ethanol water immersion 4h, after centrifuge impurity elimination dry, meal must be dried；
S2, in mass ratio 2:0.5, will dry after meal is mixed with coal tar in addition regeneration reactor, regeneration 18h
Afterwards, tire devulcanized rubber must be reclaimed；
S3, the poly- methyl vinyl silicone rubber of the HMW of the proportion and recovery tire devulcanized rubber are added and is mediated
In machine, kneaded at a high temperature of 150 DEG C, sequentially added surfactant, nano titanium oxide, liquid silastic and fire-retardant
Agent, is mixed when adding with the rotating speed of 150r/min, and 55 DEG C of insulations are cooled to after mixing 10h, obtains blend glue stuff；
S4, the perbenzoic acid of the proportion is added in the compound being incubated in step S3, continues to stir mixing
25min, using double screw extruder, the extruding pelletization at 145 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
Embodiment three
A kind of Black flame-retardant silicon rubber material proposed by the present invention, including following weight portion raw material：HMW it is poly-
60 parts of methyl vinyl silicone rubber, reclaim 50 parts of tire devulcanized rubber, 3 parts of nano titanium oxide, 5 parts of methyl ethyl ketone peroxide,
2.5 parts of surfactant, 5 parts of structure inhibitor, 3 parts of liquid silastic, 5 parts of fire retardant.
Its preparation method, comprises the following steps：
S1, waste tire is broken into tire meal, is cleaned using 60 DEG C of running water, be then 75% with concentration
Ethanol water immersion 8h, after centrifuge impurity elimination dry, meal must be dried；
S2, in mass ratio 3:0.4, will dry after meal is mixed with coal tar in addition regeneration reactor, regeneration 22h
Afterwards, tire devulcanized rubber must be reclaimed；
S3, the poly- methyl vinyl silicone rubber of the HMW of the proportion and recovery tire devulcanized rubber are added and is mediated
In machine, kneaded at a high temperature of 200 DEG C, sequentially added surfactant, nano titanium oxide, liquid silastic and fire-retardant
Agent, is mixed when adding with the rotating speed of 300r/min, and 70 DEG C of insulations are cooled to after mixing 6h, obtains blend glue stuff；
S4, the methyl ethyl ketone peroxide of the proportion is added in the compound being incubated in step S3, continues to stir mixed
50min is closed, using double screw extruder, the extruding pelletization at 128 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
Example IV
A kind of Black flame-retardant silicon rubber material proposed by the present invention, including following weight portion raw material：HMW it is poly-
55 parts of methyl vinyl silicone rubber, 30 parts of recovery tire devulcanized rubber, 1 part of nano titanium oxide, 3 parts of tert-butyl peroctoate, table
3 parts of face activating agent, 2 parts of structure inhibitor, 5 parts of liquid silastic, 3 parts of fire retardant.
Its preparation method, comprises the following steps：
S1, waste tire is broken into tire meal, is cleaned using 55 DEG C of running water, be then 70% with concentration
Ethanol water immersion 7h, after centrifuge impurity elimination dry, meal must be dried；
S2, in mass ratio 75:0.4, will dry after meal is mixed with coal tar in addition regeneration reactor, regeneration
After 24h, tire devulcanized rubber must be reclaimed；
S3, the poly- methyl vinyl silicone rubber of the HMW of the proportion and recovery tire devulcanized rubber are added and is mediated
In machine, kneaded at a high temperature of 120 DEG C, sequentially added surfactant, nano titanium oxide, liquid silastic and fire-retardant
Agent, is mixed when adding with the rotating speed of 100r/min, and 65 DEG C of insulations are cooled to after mixing 9h, obtains blend glue stuff；
S4, the tert-butyl peroctoate of the proportion is added in the compound being incubated in step S3, continues to stir mixing
30min, using double screw extruder, the extruding pelletization at 140 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
Embodiment five
A kind of Black flame-retardant silicon rubber material proposed by the present invention, including following weight portion raw material：HMW it is poly-
40 parts of methyl vinyl silicone rubber, 45 parts of recovery tire devulcanized rubber, 2.5 parts of nano titanium oxide, 2 parts of peroxide sulphonyl class, table
1.5 parts of face activating agent, structure inhibitors 4 part, 4 parts of liquid silastic, 5 parts of fire retardant.
Its preparation method, comprises the following steps：
S1, waste tire is broken into tire meal, is cleaned using 75 DEG C of running water, be then 85% with concentration
Ethanol water immersion 6h, after centrifuge impurity elimination dry, meal must be dried；
S2, in mass ratio 4:0.5, will dry after meal is mixed with coal tar in addition regeneration reactor, regeneration 20h
Afterwards, tire devulcanized rubber must be reclaimed；
S3, the poly- methyl vinyl silicone rubber of the HMW of the proportion and recovery tire devulcanized rubber are added and is mediated
In machine, kneaded at a high temperature of 160 DEG C, sequentially added surfactant, nano titanium oxide, liquid silastic and fire-retardant
Agent, is mixed when adding with the rotating speed of 250r/min, and 50 DEG C of insulations are cooled to after mixing 7h, obtains blend glue stuff；
S4, the peroxide sulphonyl class of the proportion is added in the compound being incubated in step S3, continues to stir mixing
45min, using double screw extruder, the extruding pelletization at 135 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
Performance test is carried out to Black flame-retardant silicon rubber material prepared by above-described embodiment one~five respectively, following knot is drawn
Really：
| Embodiment | One | Two | Three | Four | Five |
| Tensile strength | 15MPa | 12MPa | 18MPa | 13MPa | 16MPa |
| Elongation at break | 520 | 498 | 505 | 514 | 523 |
| Tearing strength | 48N/mm | 51N/mm | 43N/mm | 45N/mm | 50N/mm |
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (8)
1. a kind of Black flame-retardant silicon rubber material, it is characterised in that the raw material including following weight portion：40~60 parts of rubber, benefit
Strong 30~50 parts of filler, 1~3 part of nano titanium oxide, 2~5 parts of vulcanizing agent, 1~3 part of surfactant, structure inhibitor 2~
5 parts, 3~8 parts of adhesive, 2~5 parts of fire retardant.
2. a kind of Black flame-retardant silicon rubber material according to claim 1, it is characterised in that the original including following weight portion
Material：45~55 parts of rubber, 35~45 parts of reinforced filling, 1.5~2.5 parts of nano titanium oxide, 3~4 parts of vulcanizing agent, surface-active
1.5~2.5 parts of agent, 3~4 parts of structure inhibitor, 4~7 parts of adhesive, 3~4 parts of fire retardant.
3. a kind of Black flame-retardant silicon rubber material according to claim 1, it is characterised in that the original including following weight portion
Material：50 parts of rubber, 40 parts of reinforced filling, 2 parts of nano titanium oxide, 3.5 parts of vulcanizing agent, 2 parts of surfactant, structure inhibitor
3.5 parts, 5 parts of adhesive, 3.5 parts of fire retardant.
4. a kind of Black flame-retardant silicon rubber material according to claim 1, it is characterised in that the rubber is HMW
Poly- methyl vinyl silicone rubber.
5. a kind of Black flame-retardant silicon rubber material according to claim 1, it is characterised in that the reinforced filling is to reclaim
Tire devulcanized rubber.
6. a kind of Black flame-retardant silicon rubber material according to claim 1, it is characterised in that the vulcanizing agent is peroxidating
In benzoic acid, excessively sad tert-pentyl ester, tert-butyl peroctoate, methyl ethyl ketone peroxide, peroxide sulphonyl class and ketal peroxide class
One or more.
7. a kind of Black flame-retardant silicon rubber material according to claim 1, it is characterised in that described adhesive is liquid silicon
Rubber.
8. a kind of preparation method of Black flame-retardant silicon rubber material, it is characterised in that comprise the following steps：
S1, waste tire is broken into tire meal, is cleaned using 55~75 DEG C of running water, then with concentration be 68~
85% ethanol water soaks 4~8h, is dried after centrifuge impurity elimination, must dry meal；
S2, in mass ratio 2~5:0.3~0.5, will dry after meal is mixed with coal tar in addition regeneration reactor, then
After raw 18~24h, reinforced filling is obtained；
S3, the rubber of the proportion and reinforced filling add kneader, kneaded at a high temperature of 120~200 DEG C, according to
Secondary addition surfactant, nano titanium oxide, adhesive and fire retardant, are entered when adding with the rotating speed of 100~300r/min
Row is mixed, and 50~70 DEG C of insulations are cooled to after 6~10h of mixing, obtains blend glue stuff；
S4, the vulcanizing agent of the proportion is added in the compound being incubated in step S3, continues to stir 25~50min of mixing,
Using double screw extruder, the extruding pelletization at 128~145 DEG C of high temperature obtains final product Black flame-retardant silicon rubber material.
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| CN201611136024.5A CN106751898A (en) | 2016-12-12 | 2016-12-12 | A kind of Black flame-retardant silicon rubber material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059830A (en) * | 2017-11-25 | 2018-05-22 | 天长市荣盛有机硅科技有限公司 | A kind of digital keys methyl vinyl silicone rubber |
| CN110387129A (en) * | 2019-06-17 | 2019-10-29 | 东莞市明盛电气有限公司 | A kind of silicone rubber wire production method |
| CN115418104A (en) * | 2022-09-01 | 2022-12-02 | 湖北工业大学 | Organic silicon slag urban step brick and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105838116A (en) * | 2016-04-01 | 2016-08-10 | 上海交通大学 | Preparation method for light-pyrolysis carbon black |
| CN106118068A (en) * | 2016-07-27 | 2016-11-16 | 苏州沃尔兴电子科技有限公司 | A kind of flame-resistant high-temperature-resistant electrically insulating silicone rubber compositions and preparation method thereof |
-
2016
- 2016-12-12 CN CN201611136024.5A patent/CN106751898A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105838116A (en) * | 2016-04-01 | 2016-08-10 | 上海交通大学 | Preparation method for light-pyrolysis carbon black |
| CN106118068A (en) * | 2016-07-27 | 2016-11-16 | 苏州沃尔兴电子科技有限公司 | A kind of flame-resistant high-temperature-resistant electrically insulating silicone rubber compositions and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108059830A (en) * | 2017-11-25 | 2018-05-22 | 天长市荣盛有机硅科技有限公司 | A kind of digital keys methyl vinyl silicone rubber |
| CN110387129A (en) * | 2019-06-17 | 2019-10-29 | 东莞市明盛电气有限公司 | A kind of silicone rubber wire production method |
| CN115418104A (en) * | 2022-09-01 | 2022-12-02 | 湖北工业大学 | Organic silicon slag urban step brick and preparation method thereof |
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