CN108445144A - A method of PE reclaimed materials carbon black contents are measured using combustion method - Google Patents
A method of PE reclaimed materials carbon black contents are measured using combustion method Download PDFInfo
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- CN108445144A CN108445144A CN201810140074.3A CN201810140074A CN108445144A CN 108445144 A CN108445144 A CN 108445144A CN 201810140074 A CN201810140074 A CN 201810140074A CN 108445144 A CN108445144 A CN 108445144A
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- combustion
- carbon black
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- pyrolysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Abstract
The present invention relates to electric wire black polyethylene plastic detection technique fields, it discloses a kind of methods measuring PE reclaimed materials carbon black contents using combustion method, initial including PE samples weigh, be pyrolyzed, be pyrolyzed after weigh, burn, burn after the methods of weigh step, after the pyrolysis in weighing process, after temperature is cooled to 400 DEG C~450 DEG C in a nitrogen atmosphere, combustion tube nozzle is opened again, combustion boat is dragged to cooling 5min at nozzle, combustion boat is taken out from combustion tube.The temperature when present invention leads to oxygen by change burning method or the soaking time at 600 DEG C when logical nitrogen, or change burning method lead to oxygen when temperature, it is promoted to 850 DEG C of logical oxygen by 600 DEG C of logical oxygen, the accuracy of the carbon black content in detection PE reclaimed materials is improved, and makes it almost the same with the testing result of thermogravimetry.
Description
Technical field
The present invention relates to electric wire black polyethylene plastic detection technique fields, and in particular to a kind of to use combustion method
The method for measuring PE reclaimed materials carbon black contents.
Background technology
In the prior art, in vinyon (PE) carbon black content detection method, mainly have thermogravimetry with burning
Two kinds of method.For example, National Standard of the People's Republic of China GB/T2951.41 (cable and the general examination of optical cable insulating and sheath material
The 41st part of proved recipe method) in define thermogravimetry and the examination criteria of combustion method.
But when using both different methods of thermogravimetry and combustion method to be detected, both institute's measured data
There is certain error, makes PE material especially for reclaimed materials, use the carbon black content number for the PE reclaimed materials that combustion method measures
It is obviously bigger than normal than the data that thermogravimetry measures according to meeting.Generally use thermogravimetry is differed with the result that combustion method measures
10% or so.Therefore, how so that the data error reduction surveyed with gravitational thermal analysis method using combustion method institute's measured data, is institute
There is the big problem that manufacturer faces.
In order to solve the above-mentioned technical problem, we analyze the characteristic of existing PE reclaimed materials, are obtained according to analysis result
Know：Completely new material PE decomposition concentrates on 450-550 DEG C, and 400-600 DEG C of concentration of reclaimed materials is decomposed, while at 600-850 DEG C
There are some other substances in some substance decomposition reclaimed materials so that reclaimed materials is at 400-600 DEG C and 600-850 DEG C
It can decompose.And use the upper limit of the pyrolysis temperature of combustion method for 600 DEG C in the prior art, and the heat preservation in pyrolytic process
Time is shorter (being that soaking time is 10min after being warming up to 600 DEG C in GB/T2951.41 standards) so that the pyrolysis of PE reclaimed materials
Process is not thorough enough, causes the carbon black content data of the PE reclaimed materials finally measured using combustion method bigger than normal.
In addition, in the prior art when the carbon black content for carrying out PE material measures, PE samples are filled after high temperature pyrolysis
The combustion boat of PE samples is higher by the temperature taken out in the combustion tube containing nitrogen, leads to the carbon black ingress of air in PE samples
It can be by an oxidation part so that carbon black content detection error increases,
Invention content
It is an object of the invention to by the specificity analysis to existing PE reclaimed materials, propose a kind of using combustion method measurement PE
The method of reclaimed materials carbon black content, it is intended to overcome and exist in the prior art in combustion method detection PE reclaimed materials content of carbon black methods
Defect, improve PE reclaimed materials content of carbon black detection accuracy, and make using combustion method and thermogravimetry method inspection
Survey result as close possible to.Specific technical solution is as follows：
A method of PE reclaimed materials carbon black contents, including following method and step are measured using combustion method：
Step 1: initially weighing：It weighs after combustion boat is dried, PE samples to be detected is put into the combustion boat after drying
Inside weigh together；
Step 2: pyrolysis：Combustion boat equipped with PE samples is put into combustion tube, be passed through in combustion tube nitrogen and be put into plus
In hot stove, the PE samples are pyrolyzed under the pyrolysis temperature of setting；
Step 3: weighing after pyrolysis：Combustion tube is taken out out of heating furnace, is opened combustion tube after cooling, taking-up is equipped with
The combustion boat of PE samples is weighed；
Step 4: burning：Combustion boat equipped with PE samples is reentered into combustion tube, air or oxygen is passed through burning
In pipe, the residual carbon black in PE samples is made to burn under the heating temperature of setting；
Step 5: weighing after burning：Combustion boat is taken out from combustion tube after burning, is weighed after cooling；
Step 6: according to the weight before and after PE sample combustions, the content of carbon black of PE samples is determined；
After the pyrolysis of the step 3 in weighing process, after temperature is cooled to 400 DEG C~450 DEG C in a nitrogen atmosphere, then
Combustion tube nozzle is opened, combustion boat is dragged to cooling 5min at nozzle, combustion boat is taken out from combustion tube.
After pyrolysis in above-mentioned measurement method in weighing process, use temperature in a nitrogen atmosphere be cooled to 400 DEG C~
Then 450 DEG C of measure again opens combustion tube nozzle, combustion boat is dragged at nozzle cooling 5min, by combustion boat from burning
It is taken out in pipe.Compared with measurement method in the prior art, PE samples of the invention pyrolysis after from combustion tube take out before by
In have passed through cooling appropriate so that its is relatively low for taking-out temperature from combustion tube for combustion boat, to effectively reduce PE samples
In carbon black oxidation by air probability, improve the accuracy of detection.
As the first improvement project to above-mentioned measurement method, in the pyrolytic process of the step 2, the setting
Pyrolysis temperature is 600 DEG C, at 600 DEG C in a nitrogen atmosphere holding time to 50min.
The first above-mentioned improvement project is due to extending the soaking time under nitrogen atmosphere, so that the pyrolysis of PE samples
It is more thorough, to further improve the accuracy of detection.
As the further preferred embodiment for the first above-mentioned improvement project, weigh after the pyrolysis of the step 3
In the process, the cooling temperature is 450 DEG C, and combustion boat cools down 10~20min after being taken out in combustion tube in drier
It weighs again；In the combustion process of the step 4, logical oxygen is warming up to 580~620 DEG C；It weighs after the burning of the step 5
In the process, by combustion boat after being taken out in combustion tube, cooling 10~20min weighs again in drier.
As second of improvement project to above-mentioned measurement method, in the pyrolytic process of the step 2, the setting
The upper limit of pyrolysis temperature is 850 DEG C, and leads to nitrogen at 0~850 DEG C；In the combustion process of the step 4, PE samples are led to
Oxygen is warming up to 850 DEG C；After the pyrolysis of the step 3 in weighing process, when temperature is reduced to 450 DEG C by 850 DEG C, by combustion boat
It is dragged to nozzle, cooling 5min weighs until being cooled to room temperature in drier.
In above-mentioned second of improvement project, the temperature that the upper limit of pyrolysis temperature and logical oxygen heat up is improved to 850 DEG C, and it is existing
There is the method that the combustion method of technology measures PE carbon black contents to compare, due to the raising of pyrolysis temperature so that the pyrolysis of PE is more thorough
Bottom, to further improve the accuracy of detection；Meanwhile set pyrolysis temperature and thermogravimetry in second of improvement project
Pyrolysis temperature it is identical, so as to realize the consistency as far as possible of combustion method and thermogravimetry measurement result, both reduce detection
As a result difference.Meanwhile since temperature is reduced to 450 DEG C by 850 DEG C again after high temperature pyrolysis in this measurement method, then will burning
Boat takes out, and taking-out temperature is relatively low, to effectively reduce the probability of the carbon black oxidation by air in PE samples, further carries
The high accuracy of detection.
In above-mentioned second of improvement project, in the combustion process of the step 4, the heating temperature that sets is 830~870
DEG C, air or oxygen is led to fitting fixed flow velocity in combustion tube at a temperature of 830~870 DEG C, residual carbon black is made to burn；Institute
It states after the burning of step 5 in weighing process, combustion boat is taken out from combustion tube, cooling 10~20min in drier, into
Row is weighed.
The beneficial effects of the invention are as follows：
First, a kind of method measuring PE reclaimed materials carbon black contents using combustion method of the invention is used in nitrogen gas
Temperature is cooled to 400 DEG C~450 DEG C of measure under atmosphere, then again opens combustion tube nozzle, combustion boat is dragged to cold at nozzle
But 5min takes out combustion boat from combustion tube.Compared with measurement method in the prior art, PE samples of the invention pyrolysis
Due to have passed through cooling appropriate before being taken out from combustion tube afterwards so that its is relatively low for taking-out temperature from combustion tube for combustion boat, from
And the probability of the carbon black oxidation by air in PE samples is effectively reduced, improve the accuracy of detection.
Second, a kind of method that PE reclaimed materials carbon black contents are measured using combustion method of the invention, the pyrolysis temperature of setting
Be 600 DEG C, at 600 DEG C in a nitrogen atmosphere holding time to 50min.When due to extending the heat preservation under nitrogen atmosphere
Between, so that the pyrolysis of PE samples is more thorough, to further improve the accuracy of detection.
Third, a kind of method that PE reclaimed materials carbon black contents are measured using combustion method of the invention, by the upper of pyrolysis temperature
Limit and the temperature of logical oxygen heating are improved to 850 DEG C, compared with the combustion method of the prior art measures the method for PE carbon black contents, due to
The raising of pyrolysis temperature so that the pyrolysis of PE is more thorough, to further improve the accuracy of detection；Meanwhile second
Set pyrolysis temperature is identical as the pyrolysis temperature of thermogravimetry in improvement project, so as to realize that combustion method is surveyed with thermogravimetry
The consistency as far as possible of result is measured, the difference of the two testing result is reduced.
Specific implementation mode
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more
Add and clearly demonstrate technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1：
A kind of combustion method PE reclaimed materials carbon black content method, including PE reclaimed materials it is initial weigh, be pyrolyzed, be pyrolyzed after claim
The step of weighing after weight, burning, burning, wherein be pyrolyzed in a nitrogen atmosphere at 600 DEG C, holding time to 50min,
So that temperature drops to 450 DEG C under this nitrogen atmosphere, then nozzle is opened, combustion boat is dragged to cooling 5min, atmosphere stream at nozzle
It is fast identical as existing examination criteria, then combustion boat is taken out from combustion tube, cooling 10~20min, goes forward side by side in drier
Row is weighed；Then combustion boat is put into combustion tube again, leads to air or oxygen with flow velocity appropriate at a temperature of (600 ± 20) DEG C
Into combustion tube, so that residual carbon black is burnt, again take out combustion boat from combustion tube, cooling 10~20min in drier,
It weighs again.
It is above-mentioned 600 DEG C in a nitrogen atmosphere holding time be conducive to exist the impurity in PE reclaimed materials to 50min
It is removed as far as possible in pyrolytic process.
Embodiment 2：
A kind of combustion method PE reclaimed materials carbon black content method, including PE reclaimed materials it is initial weigh, be pyrolyzed, be pyrolyzed after claim
The step of weighing after weight, burning, burning, after wherein PE reclaimed materials is pyrolyzed in a nitrogen atmosphere at 600 DEG C, holding time
To 50min, then when temperature is down to 400 DEG C by 600 DEG C, then nozzle is opened, is avoided under 600 DEG C of high temperature, PE reclaimed materials
Ingress of air and by an oxidation part, and then cause carbon black content detection inaccurate.
Embodiment 3：
A kind of combustion method PE reclaimed materials carbon black content method, including PE reclaimed materials it is initial weigh, be pyrolyzed, be pyrolyzed after claim
The step of weighing after weight, burning, burning, wherein leading to nitrogen at 0~850 DEG C will fire when temperature is reduced to 450 DEG C by 850 DEG C
It burns boat and is dragged to nozzle, cooling 5min weighs until being cooled to room temperature in drier；It will be empty at a temperature of (850 ± 20) DEG C
Gas or oxygen are led to flow velocity appropriate in combustion tube, so that residual carbon black is burnt, are again taken out combustion boat from combustion tube,
Cooling 10~20min, weighs again in drier.
Lead to nitrogen at above-mentioned 0~850 DEG C so that its pyrolysis temperature condition and the pyrolysis temperature condition of gravitational thermal analysis method are protected
It holds consistent.
It is above-mentioned that temperature in pipe is dropped to 450 DEG C after 850 DEG C of high temperature pyrolysis, can be to avoid under 850 DEG C of high temperature, PE is returned
Rewinding ingress of air and by an oxidation part, and then cause carbon black content detection inaccurate.
Embodiment 4：
Certain batch of PE reclaimed materials is sampled, and the sample of PE reclaimed materials is divided into two groups, first group using using implementation
The combustion method of example 3 carries out carbon black content detection, and second group is detected using thermogravimetry, as a result as follows：
The carbon black content that the combustion method of embodiment 3 measures is used to be measured using thermogravimetry for 2.31~2.37%
Carbon black content is 2.18~2.33%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (5)
1. a kind of method measuring PE reclaimed materials carbon black contents using combustion method, which is characterized in that including following method and step：
Step 1: initially weighing：It weighs after combustion boat is dried, PE samples to be detected is put into one in the combustion boat after drying
It rises and weighs；
Step 2: pyrolysis：Combustion boat equipped with PE samples is put into combustion tube, nitrogen is passed through in combustion tube and is put into heating furnace
It is interior, the PE samples are pyrolyzed under the pyrolysis temperature of setting；
Step 3: weighing after pyrolysis：Combustion tube is taken out out of heating furnace, opens combustion tube after cooling, takes out and PE samples is housed
The combustion boat of product is weighed；
Step 4: burning：Combustion boat equipped with PE samples is reentered into combustion tube, air or oxygen is passed through combustion tube
It is interior, so that the residual carbon black in PE samples is burnt under the heating temperature of setting；
Step 5: weighing after burning：Combustion boat is taken out from combustion tube after burning, is weighed after cooling；
Step 6: according to the weight before and after PE sample combustions, the content of carbon black of PE samples is determined；
After the pyrolysis of the step 3 in weighing process, after temperature is cooled to 400 DEG C~450 DEG C in a nitrogen atmosphere, then will combustion
It burns pipe nozzle to open, combustion boat is dragged to cooling 5min at nozzle, combustion boat is taken out from combustion tube.
2. a kind of method measuring PE reclaimed materials carbon black contents using combustion method according to claim 1, which is characterized in that
In the pyrolytic process of the step 2, the pyrolysis temperature set is 600 DEG C, when being kept the temperature in a nitrogen atmosphere at 600 DEG C
Between extend to 50min.
3. a kind of method measuring PE reclaimed materials carbon black contents using combustion method according to claim 2, which is characterized in that
After the pyrolysis of the step 3 in weighing process, the cooling temperature be 450 DEG C, and combustion boat from combustion tube take out after,
Cooling 10~20min weighs again in drier；In the combustion process of the step 4, logical oxygen is warming up to 580~
620℃；It is cold in drier by combustion boat after being taken out in combustion tube after the burning of the step 5 in weighing process
But 10~20min weighs again.
4. a kind of method measuring PE reclaimed materials carbon black contents using combustion method according to claim 1, which is characterized in that
In the pyrolytic process of the step 2, the upper limit of the pyrolysis temperature set leads to nitrogen at 0~850 DEG C as 850 DEG C；
In the combustion process of the step 4, PE samples are led into oxygen and are warming up to 850 DEG C；After the pyrolysis of the step 3 in weighing process,
When temperature is reduced to 450 DEG C by 850 DEG C, combustion boat is dragged to nozzle, cooling 5min is carried out until being cooled to room temperature in drier
It weighs.
5. a kind of method measuring PE reclaimed materials carbon black contents using combustion method according to claim 4, which is characterized in that
In the combustion process of the step 4, the heating temperature set is 830~870 DEG C, by air at a temperature of 830~870 DEG C
Or oxygen is led to fitting fixed flow velocity in combustion tube, and residual carbon black is made to burn；It, will after the burning of the step 5 in weighing process
Combustion boat takes out from combustion tube, and cooling 10~20min, weighs in drier.
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Cited By (2)
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| CN110376363A (en) * | 2019-08-09 | 2019-10-25 | 义乌市婉聚电子有限公司 | A kind of equipment measuring PE reclaimed materials carbon black content |
| CN114018978A (en) * | 2021-10-09 | 2022-02-08 | 广西电网有限责任公司电力科学研究院 | Method for quantifying micro-plastic in environment based on micro-combustion calorimetry |
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| CN110376363A (en) * | 2019-08-09 | 2019-10-25 | 义乌市婉聚电子有限公司 | A kind of equipment measuring PE reclaimed materials carbon black content |
| CN114018978A (en) * | 2021-10-09 | 2022-02-08 | 广西电网有限责任公司电力科学研究院 | Method for quantifying micro-plastic in environment based on micro-combustion calorimetry |
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Application publication date: 20180824 |