CN103028581B - Handling method of sand core crucible used for detecting insoluble quinoline - Google Patents
Handling method of sand core crucible used for detecting insoluble quinoline Download PDFInfo
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Abstract
The invention discloses a handling method of a sand core crucible used for detecting insoluble quinoline insoluble. The handling method of the sand core crucible used for detecting the insoluble quinoline insoluble includes the following steps: (1) a high temperature burning step: the sand core crucible is placed in a high temperature furnace. The temperature of the high temperature furnace rises to 500 DEG C, the sand core crucible is ensured to be burned for 1.8-2.2 hours under the furnace constant temperature of 500 DEG C, then the high temperature furnace is closed and the door of the high temperature furnace is opened until the temperature of the internal furnace falls to the normal temperature, and then the sand core crucible is taken out and cools to the room temperature; (2) a steam blowing step: the sand core crucible after being burned through the high temperature is blown under a steam generator for 3-5 minutes; (3) a ultrasonic wave cleaning step: the sand core crucible after being blown through steam is moved to an ultrasonic wave cleaner to be cleaned for 8-12 minutes; (4) a drying step: first, the sand core crucible is taken out from the ultrasonic wave cleaner and is washed through distilled water, and then is moved inside a constant temperature drying box with 120+-1 DEG C to be dried for 0.8-1.2 hours. The handling method of the sand core crucible used for detecting the insoluble quinoline is capable of ensuring that the sand core crucible after being used can be handled conveniently, fast and completely in an environment-friendly mode.
Description
Technical field
The present invention relates to the processing method after a kind of chemical analysis equipment is used, be specifically related to a kind of processing method of the core crucible for detection of quinoline insolubles.
Background technology
The method that the quinoline insolubles employing in oils sample is detected in laboratory is core filtration method.Core crucible is to detect to analyze the quantitative analysis utensil that quinoline insolubles is used.
Core crucible system selects porous ceramics raw material and glass to form through high temperature sintering.Core sheet has many fine holes, is the shank of performance filtration, and the filtration by sand filtration chip obtains required analysis result.
Detect under normal circumstances all transducer set filter cores more of more than ten batches of sample, if but the analytical sample of encountering is very special needle-like oils sample, in practical operation, almost analyze the filter opening that uses a core sheet just blocked and cannot continue to use.This is due to after the quinoline insolubles of core crucible in having analyzed heavy oils sample, can on the surface of bottom core sheet, pile up one deck organic impurities and inorganic impurity, organic impurities is the γ resin that is insoluble to quinoline, inorganic impurity is mostly black carbon powder or other impurity, these impurity are that a kind of very tiny particle packing is on core sheet, if do not do effective removing, core crucible just can not reuse.General stopping state has two kinds, and a kind of is that mechanical admixture stops up, and another kind is product Crystallization Plugging.And that often run at present is the former.In order to prevent Particle Blocking filter opening, conventionally carry out conventional processing method three times, before filtration, sample is carried out to pre-filtering, if what use such as ortho-test is the core sheet of 1u, the filter element slice that can add 10u before filtration carries out pre-filtering.Yet the sample of analyzing due to laboratory is the sample containing micro-quinoline insolubles, be that sticky oil impurities and particle are minimum mostly, carrying out pre-filtering does not have positive effect, and has greatly increased analytical error.
Because the detection frequency of laboratory quinoline insolubles is quite high, often within one day, can detect more than ten quinoline insolubles, as the core after using is discarded with rear, will greatly increase analysis cost.Therefore, urgently find a kind of processing method of core recycling to reduce analysis cost, improve analysis efficiency.
Summary of the invention
The object of the invention is in order to overcome the deficiencies in the prior art, a kind of processing method of the core crucible for detection of quinoline insolubles is provided, it can be convenient, fast, thoroughly, the core crucible after using is processed on environmental protection ground, core crucible after using and new core crucible can reach same detection effect, and core crucible can be recycled.
A kind of technical scheme that realizes above-mentioned purpose is: a kind of processing method of the core crucible for detection of quinoline insolubles, comprises the following steps:
High temperature sintering step, first described core crucible is placed in to high temperature furnace, the temperature of high temperature furnace is risen to 500 ℃, make the aerobic constant temperature calcination 1.8～2.2 hours under the furnace temperature of 500 ℃ of described core crucible, close again high temperature furnace and open fire door, make fire box temperature slowly be down to normal temperature, then take out core crucible and be cooled to room temperature;
Steam blowing step purges 3～5 minutes by the core crucible after high temperature sintering under steam generator;
Ultrasonic Cleaning step, moves into the core crucible after steam blowing in supersonic wave cleaning machine and cleans 8～12 minutes;
Drying steps first takes out core crucible from supersonic wave cleaning machine, clean with distilled water flushing, then moves into the thermostatic drying chamber inner drying 0.8～1.2 hour of 120 ± 1 ℃.
The processing method of the above-mentioned core crucible for detection of quinoline insolubles, wherein, when carrying out described high temperature sintering step, described high-temperature furnace door leaves the gap of 8～12mm, makes in described high temperature furnace high temperature sintering under aerobic state.
The processing method of the above-mentioned core crucible for detection of quinoline insolubles, wherein, when carrying out described steam blowing step, adopts wood clamp or bamboo tweezer to clamp described core crucible and carries out.
The processing method of the above-mentioned core crucible for detection of quinoline insolubles, wherein, when carrying out described Ultrasonic Cleaning step, described supersonic wave cleaning machine uses pure water as cleaning fluid, and hyperacoustic vibration frequency is greater than 20,000 hertz.
The technical scheme of the processing method of the core crucible for detection of quinoline insolubles of the present invention, the cleaning method that mainly adopts high temperature sintering and ultrasonic wave to combine, can access used core crucible and processes timely and can reuse; Whole processing procedure is nursed without personnel, and easy and simple to handle; When cleaning, without using chemical reagent, can process the core crucible after using in environmental protection ground, the core crucible after using and new core crucible can reach same detection effect, can make core crucible recycle.
The specific embodiment
Below by specific embodiment, technical scheme of the present invention is elaborated:
The processing method of a kind of core crucible for detection of quinoline insolubles of the present invention, comprises the following steps:
High temperature sintering step, first core crucible is placed in to high temperature furnace, the temperature of high temperature furnace is risen to 500 ℃, make the aerobic constant temperature calcination 1.8～2.2 hours under the furnace temperature of 500 ℃ of core crucible, close again high temperature furnace and open fire door, make fire box temperature slowly be down to normal temperature, then take out core crucible and be cooled to room temperature; During calcination, fire door is left to the gap of 10mm, make in high temperature furnace high temperature sintering under aerobic state, the organic impurities and the inorganic impurity that make to stay on the core sheet of core crucible bottom change into carbon dioxide, i.e. C-H-O+O
2→ CO
2↑
C+O
2→CO
2↑
Steam blowing step, because core crucible resistance to falls, resistance to insufficient strength of beaing, in order to remove the impurity such as incinerated organic matter of sand chip surface, the core crucible that adopts wood clamp or bamboo tweezer to clamp after high temperature sintering purges 3～5 minutes under steam generator;
Ultrasonic Cleaning step, moves into the core crucible after steam blowing to use pure water in the supersonic wave cleaning machine of cleaning fluid, to clean 8～12 minutes; Because hyperacoustic vibration frequency is more than 20,000 hertz, the micro-wave producing is referred to as " cavitation phenomenon " physically, constantly produce rapidly the shock wave forming with the little cavity of vanishing and as " small brushes ", wash away the surface of core sheet, so within a short period of time just can be clean by the surface clean of core sheet; The effect of Ultrasonic Cleaning is that the inorganic particle class impurity generating on core sheet after high temperature sintering is effectively departed under hyperacoustic effect;
Drying steps first takes out core crucible from supersonic wave cleaning machine, clean with distilled water flushing, then moves into the thermostatic drying chamber inner drying 0.8～1.2 hour of 120 ± 1 ℃, can reuse.
In processing method of the present invention, high temperature sintering step is a committed step.After core crucible uses, in oils sample, the quinoline insolubles of filtering is in the sand chip surface accumulation of core crucible bottom, because quinoline insolubles is organic compound, in high temperature furnace, aerobic calcination meeting is decomposed, and generates the gases such as the fine particle of some inorganic matters and carbon dioxide.Because the adhesive that core sheet is quartz sand and resistance to uniform temperature is made, its filter bores has strict restriction to the granularity by material, key is that temperature can not be too high when calcination, due to the principle of expanding with heat and contract with cold, excess Temperature can destroy the filter opening of core sheet, even can make core sheet damage, and as too low in calcination temperature, the particulate that can make to stop up the filter opening of core sheet cannot be ashed, and does not have the effect of the filter opening of dredging core sheet.Therefore, strictly control calcination temperature.According to the character of quinoline insolubles, the material that stops up the filter opening of core sheet is generally organic resin or some coal dusts, and these materials can be ashed under certain high temperature, after ashing, will carry out separated with the filter opening of core sheet, so again through the processing of steam blowing and Ultrasonic Cleaning two steps subsequently, core crucible can processedly totally also can utilize completely again.
Below the effect that adopts one group of core crucible after disposal methods of the present invention and one group of new core crucible to measure the content of quinoline insolubles in same coal tar is compared, obtains following table:
In above-mentioned table:
1. by the precision that homogeneity test of variance method F checks new and old core crucible to measure quinoline insolubles content in same coal tar sample, whether there is significant difference:
Selected level of significance α=0.05
Look into the F check table of corresponding α value, the free degree is (5,5) corresponding F α=5.05
Due to F
0< F α, the precision of two group analysis data is that 100 (1-α)=95% time are consistent at confidence level, must make new advances, the precision of quinoline insolubles content does not exist conspicuousness error in the same coal tar sample of old sand core crucible assay;
2. in two kinds of same coal tar samples of core crucible assay of check, whether the degree of accuracy of quinoline insolubles content has significant difference:
Selected level of significance α=0.05
Look into t check critical value: free degree f=n1+n2-2=6+6-2=10, check in t
0.05,10=1.812
S: be sample standard deviation, represent the dispersion degree of sample parameter,
I: the natural number from 1 to n,
sample mean
N: number of samples
Due to t < t
0.05,10=1.812, so there is not systematic error in these two kinds of methods.
Conclusion: in two kinds of same coal tar samples of core crucible assay, quinoline insolubles content does not have a significant difference.Newly, old sand core crucible can reach same analytical effect.
Those of ordinary skill in the art will be appreciated that, above embodiment is only for the present invention is described, and be not used as limitation of the invention, as long as within the scope of connotation of the present invention, to the variation of the above embodiment, modification, all will drop within the scope of claims of the present invention.
Claims (4)
1. for detection of a processing method for the core crucible of quinoline insolubles, it is characterized in that, the treating method comprises following steps:
High temperature sintering step, first described core crucible is placed in to high temperature furnace, the temperature of high temperature furnace is risen to 500 ℃, make the aerobic constant temperature calcination 1.8～2.2 hours under the furnace temperature of 500 ℃ of described core crucible, close again high temperature furnace and open fire door, make fire box temperature slowly be down to normal temperature, then take out core crucible and be cooled to room temperature;
Steam blowing step purges 3～5 minutes by the core crucible after high temperature sintering under steam generator;
Ultrasonic Cleaning step, moves into the core crucible after steam blowing in supersonic wave cleaning machine and cleans 8～12 minutes;
Drying steps first takes out core crucible from supersonic wave cleaning machine, clean with distilled water flushing, then moves into the thermostatic drying chamber inner drying 0.8～1.2 hour of 120 ± 1 ℃.
2. the processing method of the core crucible for detection of quinoline insolubles according to claim 1, is characterized in that, when carrying out described high temperature sintering step, high-temperature furnace door leaves the gap of 8～12mm, makes in described high temperature furnace high temperature sintering under aerobic state.
3. the processing method of the core crucible for detection of quinoline insolubles according to claim 1, is characterized in that, when carrying out described steam blowing step, adopts wood clamp or bamboo tweezer to clamp described core crucible and carries out.
4. the processing method of the core crucible for detection of quinoline insolubles according to claim 1, it is characterized in that, when carrying out described Ultrasonic Cleaning step, described supersonic wave cleaning machine uses pure water as cleaning fluid, and hyperacoustic vibration frequency is greater than 20,000 hertz.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109500015A (en) * | 2018-11-02 | 2019-03-22 | 云南省粮油科学研究院（云南省粮油产品质量监督检验测试中心） | A kind of cleaning method not measuring small-bore glassware internal grease |
| CN110386601B (en) * | 2019-06-24 | 2022-09-16 | 鞍钢股份有限公司 | Method for removing quinoline insoluble particles on surface of carbon microsphere |
| CN111482423A (en) * | 2020-04-08 | 2020-08-04 | 四川富乐德科技发展有限公司 | Cleaning regeneration method of titanium crucible |
| CN112834382A (en) * | 2021-04-06 | 2021-05-25 | 枣庄杰富意振兴化工有限公司 | Method for detecting content of quinoline insoluble substances |
| CN114682589A (en) * | 2022-04-11 | 2022-07-01 | 云南磷化集团有限公司 | Method for washing quinoline phosphomolybdate precipitate remained in glass sand core crucible |
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| US4028137A (en) * | 1974-11-14 | 1977-06-07 | Wacker-Chemitronic Gesellschaft Fur Elektronik-Grundstoffe Mbh | Process for the quantitative removal of residual melts from crucibles |
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Effective date of registration: 20170531 Address after: 016011 thousand mile Mountain Industrial Park, Haibowan District, the Inner Mongolia Autonomous Region, Wuhai Patentee after: WUHAI BAOHUA WANCHEN COAL CHEMICAL CO.,LTD. Address before: 200942 Baoshan District Shanghai Baoshan Iron and steel plant in the area of chemical office building road, three Patentee before: Shanghai Baosteel Chemical Co.,Ltd. |
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Address after: 016000 QIANLISHAN Industrial Park, Haibowan District, Wuhai City, Inner Mongolia Autonomous Region Patentee after: Wuhai Baoqi Carbon Materials Co.,Ltd. Address before: 016011 QIANLISHAN Industrial Park, Haibowan District, Wuhai City, Inner Mongolia Autonomous Region Patentee before: WUHAI BAOHUA WANCHEN COAL CHEMICAL CO.,LTD. |