CN105784452A - Method for extracting and separating carbon black from vulcanized rubber - Google Patents
Method for extracting and separating carbon black from vulcanized rubber Download PDFInfo
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- CN105784452A CN105784452A CN201410785904.XA CN201410785904A CN105784452A CN 105784452 A CN105784452 A CN 105784452A CN 201410785904 A CN201410785904 A CN 201410785904A CN 105784452 A CN105784452 A CN 105784452A
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- carbon black
- vulcanizate
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- vulcanized rubber
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Abstract
The invention discloses a method for extracting and separating carbon black from vulcanized rubber. The method comprises the following steps: cutting the vulcanized rubber to form small particles, and cracking the small particles under the protection of nitrogen to remove organic ingredients and rubber from the vulcanized rubber; grinding residues to obtain fine powder, transferring the fine powder to a platinum crucible, adding hydrofluoric acid, and heating the crucible under the protection of water to remove silica and acid-soluble metal oxides and carbonates; and carrying out microwave digestion on the processed residues to remove alumina. Carbon black is extracted and separated through above treatments. The method allows the carbon black to be extracted and separated on the premise of guaranteeing of carbon black invariance and less loss, and makes preparations for further researches.
Description
Technical field:
The present invention relates to the formulation analysis field of vulcanizate, be specifically related to a kind of method extracting separating off carbon black from vulcanizate, it is possible to as the pre-treating method of kind of carbon black discriminating work in vulcanizate.
Technical background:
In general, tire and rubber comprise organic compounding ingredient, rubber hydrocarbon, white carbon black, this four part of inorganic filler.The anatomy of its formula refers to qualitatively and quantitatively to be analyzed this tetrameric composition, wherein the qualitative analysis of white carbon black is referred to and the kind of white carbon black in vulcanizate is differentiated.Extracting separating off carbon black from vulcanizate is exactly the organic compounding ingredient in removing vulcanizate, rubber hydrocarbon and inorganic filler under the premise guaranteeing white carbon black invariance, finally gives the process of white carbon black.This process can as the pre-treatment that the kind of white carbon black is differentiated.Current existing white carbon black extraction separation method is method described in GB/T7766-2000 " in rubber the mensuration nitric acid digestion method of content of carbon black ", organic compounding ingredient in rubber is removed by the mode of extracting by the method first with organic solvent, afterwards residue nitric acid etc. is carried out digestion process when heating in water bath boils, finally postdigestive residue is filtered, hot nitric acid is washed, organic solvent is washed, thermohaline pickling, drying, finally give white carbon black.The method is disadvantageous in that and cannot silicon dioxide, aluminium sesquioxide be separated with white carbon black.But silicon dioxide is widely used in vulcanite as a kind of important reinforcing agent, the tyre surface position etc. of such as tire；Aluminium sesquioxide can play fire-retardant in rubber and strengthen bubble-tight effect, applies also comparatively general.Therefore, the method is not suitable for the rubber product containing silicon dioxide, aluminium sesquioxide.Additionally, the inadequate environmental protection of reagent such as the organic solvent used in the method, strong acid are also safe not.
The invention provides a kind of method extracting separating off carbon black from vulcanizate, under the premise not changing white carbon black character, white carbon black is extracted from vulcanizate, and make white carbon black separate with silicon dioxide, aluminium sesquioxide, compensate for current existing methods weak point, and this method environmental protection, safe efficient, loss is few.
Summary of the invention
It is an object of the invention to provide a kind of method extracting separating off carbon black from vulcanizate, comprise the following steps:
(1) vulcanizate is cut into little micelle, holds with porcelain boat, then cracking under high pure nitrogen is protected；
(2) residue after step (1) processes is shifted in agate mortar, be ground into fine powder；
(3) fine powder after step (2) processes is shifted in platinum crucible, add Fluohydric acid. and heat when water conservation, keeping micro-and boil, cooling down, filter, dry；
(4) sample after step (3) processes is carried out micro-wave digestion, cooling, filtration, drying.
The cracking treatment temperature of vulcanizate of the present invention is 600 DEG C；
Water conservation condition of the present invention adds deionized water after referring to addition Fluohydric acid.；
Heating of the present invention refers to maintenance slight boiling condition 20 minutes.
The invention has the beneficial effects as follows, under the premise that the white carbon black character in guaranteeing vulcanizate does not change, total amount loss is few, white carbon black is extracted from vulcanizate and separates, with for further study.
Accompanying drawing illustrates:
Fig. 1 is the process chart of the present invention.
Detailed description of the invention:
1, vulcanizate is cut into little micelle.
2, weigh in the porcelain crucible that appropriate little micelle puts into constant weight.Porcelain crucible is placed on electric furnace, under ensureing the incombustible situation of sample, slowly heats, till not smoldering in crucible.Crucible is transferred in high temperature furnace, keeps furnace temperature 850 DEG C, calcination 1 hour, and reach constant weight.Take out crucible to be placed in exsiccator and stand 30 minutes, weigh.Calculate content of ashes.
3, appropriate sulfuration micelle is put in porcelain boat, porcelain boat is placed in tube furnace, under high pure nitrogen is protected, keep tubular type furnace temperature 600 DEG C, crack 20 minutes, take out, be cooled to room temperature.
4, residue after cracking is shifted in agate mortar, finely ground one-tenth powder.
If the content of ashes of 5 vulcanizates is less than 5%, then residue powder after finely ground cracking is transferred in beaker, add the hydrochloric acid of excessive 1:1 and stir, filtering with quantitative filter paper after static 20 minutes, with deionized water rinsing till the pH value of the water leached and the pH value of deionized water are identical.Filter paper and residue are shifted on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour, take out surface plate and be placed in exsiccator, be cooled to room temperature.
If the content of ashes of 6 vulcanizates is more than 5%, and ash does not have the material not reacted with Fluohydric acid., then residue powder after finely ground cracking is transferred in platinum crucible, after adding Fluohydric acid., add deionized water, be placed on electric furnace heat, keep micro-and boil 20 minutes.Platinum crucible is taken off from electric furnace, is cooled to room temperature, use quantitative filter paper filtration residue, with deionized water rinsing till the pH value of the water leached and the pH value of deionized water are identical.Filter paper and residue are placed on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour, take out surface plate and be placed in exsiccator, be cooled to room temperature.
If the content of ashes of 7 vulcanizates is more than 5%, and containing the material not reacted with Fluohydric acid., then residue powder after finely ground cracking is transferred in platinum crucible, after adding Fluohydric acid., adds deionized water, be placed on electric furnace and heat 20 minutes, keep micro-and boil.Platinum crucible is taken off from electric furnace, is cooled to room temperature, use quantitative filter paper filtration residue, with deionized water rinsing till the pH value of the water leached and the pH value of deionized water are identical.Filter paper and residue are placed on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour.Take out surface plate and be placed in exsiccator, be cooled to room temperature.Sample after drying is put into microwave dissolver, adds phosphoric acid and concentrated sulphuric acid carries out micro-wave digestion, afterwards with deionized water rinsing till the pH value of the water leached and the pH value of deionized water are identical.Filter paper and residue are placed on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour.Take out surface plate and be placed in exsiccator, be cooled to room temperature.
Further instruction is given by the examples below to the technology of the present invention
Example 1:
Vulcanizate sample A is cut into little micelle, weighs 2g(and be accurate to 0.0001g) put in the 30ml porcelain crucible of constant weight.Porcelain crucible is placed on electric furnace, under ensureing the incombustible situation of sample, slowly heats, till not smoldering in crucible.Crucible is transferred in high temperature furnace, keeps furnace temperature 850 DEG C, calcination 1 hour, and reach constant weight.Take out crucible to be placed in exsiccator and stand 30 minutes, weigh (being accurate to 0.0001g).Calculate content of ashes less than 5%.
Weighing appropriate amount of sample A, put in porcelain boat, be placed in tube furnace by porcelain boat, under high pure nitrogen is protected, keeping tubular type furnace temperature is 600 DEG C, takes out, be cooled to room temperature after cracking 20 minutes.Residue after cracking is transferred in agate mortar, finely ground one-tenth powder.Powder after finely ground is transferred in beaker, adds the hydrochloric acid of 15ml1:1 and stir, filter with quantitative filter paper after static 20 minutes, repeatedly rinse till the pH value of the water leached and the pH value of deionized water are identical with deionized water.Filter paper and residue are transferred on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour, take out surface plate and be placed in exsiccator, be cooled to room temperature.
Example 2:
Vulcanizate sample B is cut into little micelle, weighs 2g(and be accurate to 0.0001g) put in the 30ml porcelain crucible of constant weight.Porcelain crucible is placed on electric furnace, under ensureing the incombustible situation of sample, slowly heats, till not smoldering in crucible.Crucible is transferred in high temperature furnace, keeps furnace temperature 850 DEG C, calcination 1 hour, and reach constant weight.Take out crucible to be placed in exsiccator and stand 30 minutes, weigh (being accurate to 0.0001g).Calculate content of ashes more than 5%.Ash in crucible is transferred in 30ml platinum crucible, adds 15ml Fluohydric acid., platinum crucible is placed on electric furnace and heats dryouies, platinum crucible does not have residue.Take off platinum crucible, be cooled to room temperature.
Weighing appropriate amount of sample B, put in porcelain boat, be placed in tube furnace by porcelain boat, under high pure nitrogen is protected, keeping tubular type furnace temperature is 600 DEG C, takes out, be cooled to room temperature after cracking 20 minutes.Residue after cracking is shifted in agate mortar, finely ground one-tenth powder.Powder after finely ground is transferred in platinum crucible, after adding 10ml Fluohydric acid., adds 15ml deionized water, electric furnace heats, keeps micro-and boil 20 minutes.From electric furnace, take off platinum crucible, be cooled to room temperature.Filter with quantitative filter paper, repeatedly rinse till the pH value of the water leached and the pH value of deionized water are identical with deionized water.Filter paper and residue are transferred on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour, take out surface plate and be placed in exsiccator, be cooled to room temperature.
Example 3:
Vulcanizate sample C is cut into little micelle, weighs 2g(and be accurate to 0.0001g) put in the 30ml porcelain crucible of constant weight.Porcelain crucible is placed on electric furnace, under ensureing the incombustible situation of sample, slowly heats, till not smoldering in crucible.Crucible is transferred in high temperature furnace, keeps furnace temperature 850 DEG C, calcination 1 hour, and reach constant weight.Take out crucible and put into standing 30 minutes, weigh (being accurate to 0.0001g) in exsiccator.Calculate content of ashes more than 5%.Ash in crucible is transferred in 30ml platinum crucible, adds 15ml Fluohydric acid., platinum crucible is placed on electric furnace and heats dryouies, containing residue in platinum crucible.Take off platinum crucible, be cooled to room temperature.
Weighing appropriate sample C, put in porcelain boat, be placed in tube furnace by porcelain boat, under high pure nitrogen is protected, keeping tubular type furnace temperature is 600 DEG C, takes out, be cooled to room temperature after cracking 20 minutes.Residue after cracking is shifted in agate mortar, finely ground one-tenth powder.Powder after finely ground is transferred in platinum crucible, adds 15ml deionized water after adding 10ml Fluohydric acid., electric furnace heats, keeps micro-and boil 20 minutes.From electric furnace, take off platinum crucible, be cooled to room temperature.Filter with quantitative filter paper, repeatedly rinse till the pH value of the water leached and the pH value of deionized water are identical with deionized water.Filter paper and residue are transferred on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour, take out surface plate and put in exsiccator, be cooled to room temperature.
Residue after drying is put into microwave dissolver, adds phosphoric acid and concentrated sulphuric acid carries out micro-wave digestion.Residue after micro-wave digestion quantitative filter paper filters, and repeatedly rinses till the pH value of the water leached and the pH value of deionized water are identical with deionized water.Filter paper and residue are transferred on glass surface ware, surface plate is placed in baking oven, keep 125 DEG C of baking oven, dry 1 hour, take out surface plate and be placed in exsiccator, be cooled to room temperature.
Claims (4)
1. the method extracting separating off carbon black from vulcanizate, it is characterised in that comprise the following steps:
(1) vulcanizate is cut into little granule, cracking under high pure nitrogen is protected；
(2) residue after step (1) processes is shifted in agate mortar, be ground into fine powder；
(3) fine powder after step (2) processes is shifted in platinum crucible, add Fluohydric acid. and heat when water conservation, keeping micro-and boil, cooling down, filter, dry；
(4) sample after step (3) processes use microwave dissolver carry out micro-wave digestion process, washing, filtration, drying.
2. the method extracting separating off carbon black from vulcanizate according to claim 1, it is characterised in that in described step (1), the cracking treatment temperature of vulcanizate is 600 DEG C.
3. the method extracting separating off carbon black from vulcanizate according to claim 1, it is characterised in that in described step (3), water conservation condition adds deionized water after referring to addition Fluohydric acid..
4. the method extracting separating off carbon black from vulcanizate according to claim 1, it is characterised in that in described step (3), heating is to slight boiling condition, and keeps 20 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113484209A (en) * | 2021-05-24 | 2021-10-08 | 浦林成山（山东）轮胎有限公司 | Method for identifying white carbon black in vulcanized rubber and application thereof |
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| JPH09152398A (en) * | 1995-11-30 | 1997-06-10 | Iwasaki Electric Co Ltd | Device for testing weather resistance |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113484209A (en) * | 2021-05-24 | 2021-10-08 | 浦林成山（山东）轮胎有限公司 | Method for identifying white carbon black in vulcanized rubber and application thereof |
| CN113484209B (en) * | 2021-05-24 | 2023-08-18 | 浦林成山（山东）轮胎有限公司 | Identification method of white carbon black in vulcanized rubber and application thereof |
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