CN109932269A - A kind of test method of lead powder oil content - Google Patents
A kind of test method of lead powder oil content Download PDFInfo
- Publication number
- CN109932269A CN109932269A CN201910200404.8A CN201910200404A CN109932269A CN 109932269 A CN109932269 A CN 109932269A CN 201910200404 A CN201910200404 A CN 201910200404A CN 109932269 A CN109932269 A CN 109932269A
- Authority
- CN
- China
- Prior art keywords
- lead powder
- oil
- lead
- oil content
- container
- 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.)
- Pending
Links
Landscapes
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of test methods of lead powder oil content, comprising the following steps: lead powder is placed in container, and pure water is added；Heating stirring later；It takes supernatant liquid to be put into another container, is added dilute sulfuric acid and stands wherein, after organic solvent is added in the mixed liquor for having oil after liquid separation later, continue that liquid separation is fuel-displaced and ORGANIC SOLVENT MIXTURES；It is fuel-displaced by the way of distillation or fractionating process separation, the weight of oil is weighed, oil content in lead powder is measured.The present invention provides a kind of method for effectively detecting oil content in lead powder, this method effectively avoids the interference of other impurities in lead powder, and testing result is accurate, provides reference to the subsequent treatment process of lead powder, finally effectively improves the performance of finished product lead-acid battery.
Description
Technical field
The present invention relates to a kind of test methods of lead powder oil content, belong to incinerator burner technical field.
Background technique
Lead powder is a primary raw material in lead-acid storage battery production plate active material, and lead powder is contaminated can be great
Influence battery performance；Lead powder is that leaded 99.994% or more electrolytic lead lead button is carried out ball in the master operation of the factorial production
Mill obtains；And there are two types of the main productions of electrolytic lead lead button, one is lead pig is melted cast bar, cut later using cutter
Grain；Another kind is by the direct cold cut granulating of the lead pig of monolith；First method process is more, and the production cycle is long, and labour demand is more,
At high cost, low efficiency does not use gradually now；Second method is because directly by lead pig pelletizing, and work efficiency is high,
It is current mainstream processing method, but requirement of this method to cutter is high, hydraulic drive during cold cut, for cutter
Oil or/and lubricating oil are possible to pollute the lead button being cut into, and final contaminated oil may be mixed into lead powder.Therefore, from lead powder
Detecting micro greasy dirt content in the middle has significant impact to battery performance is further increased.Since oil content is atomic in lead powder
It is small, it is used to detect greasy dirt content micro in lead powder there is no a kind of method at present and avoids the shadow of trace impurity in lead powder simultaneously
It rings.
Summary of the invention
In order to overcome drawbacks described above, the present invention provides a kind of test methods of lead powder oil content.This method can test
The oil content of the denier oil in lead powder and avoid the interference of trace impurity in lead powder out.
To achieve the goals above, the technical solution of the present invention is as follows: a kind of test method of lead powder oil content, including it is following
Step:
The lead powder that weight is x is placed in the first container, pure water is added in the first container later, stands one section by step 1
Time；
Step 2 heats the first container and is stirred simultaneously, stops heating and standing a period of time later；
Step 3 pours into the supernatant liquid in step 2 in the first container in second container；
Step 4 is added enough dilute sulfuric acids until generating without precipitating in second container, stands later；The cold cut work of present mainstream
It further include micro lead hydroxide and basic lead carbonate, hydrogen-oxygen outside the trace impurity oil removing mainly contained in lead powder made of skill
Change lead is white amorphous precipitating in water, makes mixed liquor that muddy shape be presented, is unfavorable for observation and liquid separation；And basic lead carbonate
Specific surface area is larger, has more part that can be adsorbed onto together with oil；Therefore need to be added dilute sulfuric acid and lead hydroxide, basic carbonate
Lead reaction generates lead sulfate and forms precipitating, and lead sulfate is not adsorbed with oil.
Step 5 carries out liquid separation to the mixed liquor in step 4 using separatory funnel, by most precipitating, water and dilute sulphur
Sour mixed liquor is separated from lower layer, is added in residual mixed liquor all dissolves with the immiscible organic solvent of water by oily later, after
Continuous liquid separation, isolates organic solvent and oil mixture；
Step 6 separates the organic solvent and oil mixture that generate in step 5 using the method for distillation or fractionation, and
The weight for weighing oil is y；
Step 7, calculating oil content in lead powder is y/x*100%.
Preferably, step 2 heating in the first container outlet temperature be 80-95 DEG C (temperature mainly for keep water do not boil
In the case where rising, the oil in lead powder is precipitated, avoids influencing final test essence because the oil that water boiling leads to float on above splashes
Degree), retention time 10-20min.
Preferably, the specific gravity of dilute sulfuric acid is 1.40g/cm in step 43。
Preferably, the organic solvent is benzene or ether.
Further, a preferred embodiment is also disclosed in the application, comprising the following steps: step 1 takes 1200g lead powder to be placed in
In the first beaker of 2000ml, 1500ml pure water is added along the first walls of beaker, stands 10min；
Step 2 is placed into the first beaker on electric furnace and is heated to 90 DEG C, while stirring and maintaining 15min；
Step 3 stops heating, stands 4h, supernatant liquid is poured into the second beaker, at this time the main matter in the first beaker
For trace impurity basic lead carbonate, the lead hydroxide in water, lead powder, oil, lead powder；The main matter of supernatant liquid be water, oil,
By the basic lead carbonate of oil absorption, lead hydroxide；
Step 4, it is 1.40g/cm that specific gravity is poured into the second beaker3Dilute sulfuric acid until without precipitating generate, stand later
20min further includes micro hydrogen-oxygen outside the trace impurity oil removing mainly contained in lead powder made of the cold-cutting process of present mainstream
Change lead and basic lead carbonate, lead hydroxide is white amorphous precipitating in water, makes mixed liquor that muddy shape be presented, is unfavorable for observing
And liquid separation；And the specific surface area of basic lead carbonate is larger, has more part admixed together with oil absorption；Therefore step master
If reacting using dilute sulfuric acid with lead hydroxide, basic lead carbonate and generating lead sulfate formation precipitating, it is clear and limpid to form layering
Mixture, and lead sulfate precipitation is not adsorbed mutually with oily, and wherein lead sulfate precipitation can largely be deposited in bottom, partially can be oily
Adhesion mixing, main substance is water, unreacted dilute sulfuric acid, precipitated sulfur lead plumbate, oil, mixes in oil in the second beaker at this time
Lead sulfate precipitation；
Step 5 carries out liquid separation to the mixed liquor in step 4 using separatory funnel, by most lead sulfate precipitation, water and not
The dilute sulfuric acid mixed liquor of reaction is separated from lower layer, and in residual mixed liquor, (main matter is water, dilute sulphur in residual mixed liquor later
The lead sulfate precipitation that mixes in acid, oil and oil) in benzene be added as organic solvent all dissolve that (benzene and oil dissolve each other and to be formed for oily
Layer, and the lead sulfate precipitation of adhesion mixing is separated after benzene and oil dissolve each other, in oil is deposited to bottom, lead sulfate precipitation, water and
Dilute sulfuric acid forms lower layer), continue liquid separation, isolates benzene and oil mixture；
Step 6, by step 5 benzene and oil mixture pour into round-bottomed flask, be put into rotary evaporation instrument and distilled
Separation, isolates benzene and oil, weighs the weight of oil；
Step 7, oily weight are oil content in lead powder multiplied by 100% divided by the weight of lead powder.
Having the beneficial effect that for the application provides a kind of method for effectively detecting denier oil oil content in lead powder, should
Method effectively avoids the interference of other trace impurities in lead powder, provides reference to the subsequent treatment process of lead powder, finally effectively mentions
The performance of high finished product lead-acid battery.
Specific embodiment
Technical solution of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of test method of lead powder oil content, comprising the following steps: step 1 takes 1200g lead powder to be placed in the first of 2000ml
In beaker, 1500ml pure water is added along the first walls of beaker, stands 10min；
Step 2 is placed into the first beaker on electric furnace and is heated to 90 DEG C, while stirring and maintaining 15min；
Step 3 stops heating, stands 4h, the supernatant liquid of about 150ml is poured into the second beaker of 500ml, and at this time first
Main matter in beaker is water, lead powder, oil, the trace impurity basic lead carbonate in lead powder, lead hydroxide；Supernatant liquid
Main matter is water, oil, lead hydroxide, the basic lead carbonate adsorbed by oil；
Step 4, it is 1.40g/cm that 10ml specific gravity is poured into the second beaker3Dilute sulfuric acid, stand 20min later, step master
If being reacted using dilute sulfuric acid with basic lead carbonate, lead hydroxide and generating lead sulfate, wherein lead sulfate partly precipitated, partially oily
Absorption, main substance is water, unreacted dilute sulfuric acid, precipitated sulfur lead plumbate, oil, the sulfuric acid that adsorbs in oil in the second beaker at this time
Lead precipitating；
Step 5 carries out liquid separation to the mixed liquor in step 4 using separatory funnel, by most lead sulfate precipitation, water and not
The dilute sulfuric acid mixed liquor of reaction is separated from lower layer, and in residual mixed liquor, (main matter is water, dilute sulphur in residual mixed liquor later
The lead sulfate precipitation adsorbed in acid, oil and oil) in be added 30ml benzene as organic solvent by it is oily all dissolve (benzene and oil dissolve each other,
Upper layer is formed, lead sulfate precipitation, water and dilute sulfuric acid form lower layer), continue liquid separation, isolates benzene and oil mixture；
Step 6, by step 5 benzene and oil mixture pour into round-bottomed flask, be put into rotary evaporation instrument and distilled
Separation, isolates benzene and oil, weighs the weight 0.024g of oil；
Step 7, oil content in lead powder are as follows: 0.024/1200*100%=0.020 ‰
Embodiment 2
A kind of test method of lead powder oil content, comprising the following steps: step 1 takes 1200g lead powder to be placed in the first of 2000ml
In beaker, 1500ml pure water is added along the first walls of beaker, stands 10min；
Step 2 is placed into the first beaker on electric furnace and is heated to 80 DEG C, while stirring and maintaining 20min；
Step 3 stops heating, stands 4h, the supernatant liquid of about 200ml is poured into the second beaker of 500ml, and at this time first
Main matter in beaker is water, lead powder, oil, trace impurity basic lead carbonate and lead hydroxide in lead powder；Supernatant liquid
Main matter be water, oil, lead hydroxide, by oil absorption basic lead carbonate；
Step 4, it is 1.40g/cm that specific gravity is poured into the second beaker3Dilute sulfuric acid until without precipitating generate, stand later
20min, the step mainly utilize dilute sulfuric acid to react with basic lead carbonate, lead hydroxide and generate lead sulfate, wherein lead sulfate portion
Fractional precipitation, partially by oil adsorb, at this time in the second beaker main substance be water, unreacted dilute sulfuric acid, precipitated sulfur lead plumbate,
The lead sulfate precipitation adsorbed in oil, oil；
Step 5 carries out liquid separation to the mixed liquor in step 4 using separatory funnel, by most lead sulfate precipitation, water and not
The dilute sulfuric acid mixed liquor of reaction is separated from lower layer, and in residual mixed liquor, (main matter is water, dilute sulphur in residual mixed liquor later
The lead sulfate precipitation adsorbed in acid, oil and oil) in 30ml ether be added as organic solvent all dissolve that (ether and oil are mutual for oily
It is molten, upper layer is formed, lead sulfate precipitation, water and dilute sulfuric acid form lower layer), continue liquid separation, isolates ether and oil mixture；
Step 6, by step 5 ether and oil mixture pour into round-bottomed flask, be put into rotary evaporation instrument and steamed
Fraction from, isolate ether and oil, weigh oil weight 0.023g；
Step 7, oil content in lead powder are as follows: 0.023/1200*100%=0.019 ‰.
Liquid separation involved in embodiments herein 1, embodiment 2 is operated with the basic step of liquid separation, belongs to reality
Test the routine operation of room personnel, the step of the application in omit its concrete operations description.The operating procedure of liquid separation is: first with common
In liquid to be separated injection separatory funnel, then that jumps a queue rests on separatory funnel on funnel stand or iron stand funnel
(if you need to vibrate liquid, is then stood) in iron hoop after should sufficiently vibrating again after liquid is divided into two layers, cock is unscrewed, makes subnatant
Body flows down before unscrewing cock from filler tube, it should make on the groove or aperture alignment funnel in separatory funnel top piston
The aperture of mouth neck portion, or top piston is removed, make to communicate with atmosphere, otherwise, liquid cannot flow out from lower mouth by cock
When lower layer's liquid flow is most, cut-out tap, then again pours supernatant liquid from funnel is suitable for reading immediately.
The limitation that technical solution of the present invention is not limited to the above specific embodiments, it is all to do according to the technique and scheme of the present invention
Technology deformation out, falls within the scope of protection of the present invention.
Claims (5)
1. a kind of test method of lead powder oil content, it is characterised in that: the following steps are included:
The lead powder that weight is x is placed in the first container, pure water is added in the first container later, stands one section by step 1
Time；
Step 2 heats the first container and is stirred simultaneously, stops heating and standing a period of time later；
Step 3 pours into the supernatant liquid in step 2 in the first container in second container；
Step 4 is added enough dilute sulfuric acids until generating without precipitating in second container, stands later；
Step 5 carries out liquid separation to the mixed liquor in step 4 using separatory funnel, most precipitating, water and dilute sulfuric acid is mixed
It closes liquid to separate from lower layer, is added in residual mixed liquor is all dissolved with the immiscible organic solvent of water by oily later, continue point
Liquid isolates organic solvent and oil mixture；
Step 6 separates the organic solvent and oil mixture that generate in step 5 using the method for distillation or fractionation, and
The weight for weighing oil is y；
Step 7, calculating oil content in lead powder is y/x*100%.
2. the test method of lead powder oil content according to claim 1, it is characterised in that: the first container in step 2 heating
Outlet temperature is 80-95 DEG C, retention time 10-20min.
3. the test method of lead powder oil content according to claim 2, it is characterised in that: the specific gravity of dilute sulfuric acid in step 4
For 1.40g/cm3。
4. the test method of lead powder oil content according to claim 3, it is characterised in that: the organic solvent be benzene or
Ether.
5. the test method of lead powder oil content according to claim 1-5, it is characterised in that: including following step
It is rapid:
Step 1 takes 1200g lead powder to be placed in the first beaker of 2000ml, and 1500ml pure water is added along the first walls of beaker, stands
10min；
Step 2 is placed into the first beaker on electric furnace and is heated to 90 DEG C, while stirring and maintaining 15min；
Step 3 stops heating, stands 4h, supernatant liquid is poured into the second beaker；
Step 4, it is 1.40g/cm that specific gravity is poured into the second beaker3Dilute sulfuric acid until without precipitating generate, stand later
20min；
Step 5 carries out liquid separation to the mixed liquor in step 4 using separatory funnel, most precipitating, water and dilute sulfuric acid is mixed
It closes liquid to separate from lower layer, benzene is added in residual mixed liquor later as organic solvent by oily all dissolutions, continues liquid separation, separation
Benzene and oil mixture out；
Step 6, by step 5 benzene and oil mixture pour into round-bottomed flask, be put into rotary evaporation instrument and distilled
Separation, isolates benzene and oil, weighs the weight of oil；
Step 7, oily weight are oil content in lead powder multiplied by 100% divided by the weight of lead powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910200404.8A CN109932269A (en) | 2019-03-16 | 2019-03-16 | A kind of test method of lead powder oil content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910200404.8A CN109932269A (en) | 2019-03-16 | 2019-03-16 | A kind of test method of lead powder oil content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109932269A true CN109932269A (en) | 2019-06-25 |
Family
ID=66987402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910200404.8A Pending CN109932269A (en) | 2019-03-16 | 2019-03-16 | A kind of test method of lead powder oil content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109932269A (en) |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63121728A (en) * | 1986-11-11 | 1988-05-25 | Kanebo Ltd | Automatic oil content measuring instrument |
| CN1369338A (en) * | 2001-02-12 | 2002-09-18 | 云南弗斯特金属工业有限公司 | Process for preparing scaled metal powder |
| CN102778409A (en) * | 2012-06-05 | 2012-11-14 | 中国石油大学(北京) | Device and method used for measuring content of oil and/ or liquid water in sample |
| CN104597215A (en) * | 2015-02-10 | 2015-05-06 | 浙江海洋学院 | Method for directly measuring components in oil sludge |
| CN105364080A (en) * | 2015-12-11 | 2016-03-02 | 大连远东新材料科技有限公司 | Oil-containing metal powder treatment system |
| CN105413851A (en) * | 2015-12-11 | 2016-03-23 | 大连远东新材料科技有限公司 | Method and device for separating oil-bearing metal powder |
| US20170030885A1 (en) * | 2015-07-28 | 2017-02-02 | Hitachi, Ltd. | Oil content measurement device |
| CN107290242A (en) * | 2016-04-01 | 2017-10-24 | 上海梅山钢铁股份有限公司 | The detection method of oil content in a kind of waste oil containing metallurgical slag |
| CN207408264U (en) * | 2017-11-22 | 2018-05-25 | 陕西延长石油（集团）有限责任公司 | Quick analysis measurement device containing solid heavy oil |
| CN108181196A (en) * | 2017-11-22 | 2018-06-19 | 中国石油天然气股份有限公司 | A kind of measuring method of shale oil content |
| CN109187262A (en) * | 2018-09-19 | 2019-01-11 | 常州大学 | A kind of measuring method of oil-sand oil content |
-
2019
- 2019-03-16 CN CN201910200404.8A patent/CN109932269A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63121728A (en) * | 1986-11-11 | 1988-05-25 | Kanebo Ltd | Automatic oil content measuring instrument |
| CN1369338A (en) * | 2001-02-12 | 2002-09-18 | 云南弗斯特金属工业有限公司 | Process for preparing scaled metal powder |
| CN102778409A (en) * | 2012-06-05 | 2012-11-14 | 中国石油大学(北京) | Device and method used for measuring content of oil and/ or liquid water in sample |
| CN104597215A (en) * | 2015-02-10 | 2015-05-06 | 浙江海洋学院 | Method for directly measuring components in oil sludge |
| US20170030885A1 (en) * | 2015-07-28 | 2017-02-02 | Hitachi, Ltd. | Oil content measurement device |
| CN105364080A (en) * | 2015-12-11 | 2016-03-02 | 大连远东新材料科技有限公司 | Oil-containing metal powder treatment system |
| CN105413851A (en) * | 2015-12-11 | 2016-03-23 | 大连远东新材料科技有限公司 | Method and device for separating oil-bearing metal powder |
| CN107290242A (en) * | 2016-04-01 | 2017-10-24 | 上海梅山钢铁股份有限公司 | The detection method of oil content in a kind of waste oil containing metallurgical slag |
| CN207408264U (en) * | 2017-11-22 | 2018-05-25 | 陕西延长石油（集团）有限责任公司 | Quick analysis measurement device containing solid heavy oil |
| CN108181196A (en) * | 2017-11-22 | 2018-06-19 | 中国石油天然气股份有限公司 | A kind of measuring method of shale oil content |
| CN109187262A (en) * | 2018-09-19 | 2019-01-11 | 常州大学 | A kind of measuring method of oil-sand oil content |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276097B (en) | Processing method of high density organic process wastewater in production of amprolium hydrochloride | |
| CN106008280A (en) | Taurine preparation method | |
| CN105061311B (en) | A kind of process for refining of caprolactam | |
| CN106967017A (en) | A kind of method of mixed extractant separation of tetrahydrofuran ethanol water mixture | |
| CN105439820A (en) | Method for innocently treating organic waste liquid generated in BDO production | |
| CN108658785A (en) | The separation method of difficult separation system containing triethylamine | |
| CN105784696B (en) | The analysis determining method of each valence state sulphur in a kind of sodium aluminate solution | |
| CN104535708B (en) | Method for determination of total aluminum in aluminum-based composite slag forming agent | |
| CN109932269A (en) | A kind of test method of lead powder oil content | |
| CN115386197A (en) | O-cresol formaldehyde epoxy resin and preparation process thereof | |
| CN107082443A (en) | A kind of preparation method of solid fuel cell scandium oxide | |
| US2761880A (en) | Improved process for making alcoholic solutions of alkali-metal alkoxides | |
| CN109248715A (en) | Anion exchange resin and its preparation method and application | |
| CN105932350A (en) | Recycling method for waste lead-acid storage battery lead plaster desulphurization byproduct | |
| CN110314637A (en) | A kind of modified goethite and its preparation method and application | |
| CN106277045A (en) | The technique that a kind of titanium dioxide hydrochloric acid residue resource recycles | |
| CN107841631A (en) | The preparation method of the leachate of copper in a kind of recovery waste and old circuit board | |
| TW460309B (en) | Method for recovering acrylic acid from an acrylic acid-containing process or waste water streams | |
| CN107055501B (en) | A method of hureaulite type manganese phosphate is prepared from low grade rhodochrosite leachate | |
| CN110339592A (en) | Heavy metal ion extractant and preparation method and extracting process based on fatty acid | |
| CN204734974U (en) | Distillation plant for chemistry experiments | |
| CN201527374U (en) | Acid dissolving reaction device for measuring copper content in copper and copper alloy | |
| CN214735621U (en) | Experimental device for preparing biodiesel through ester exchange reaction | |
| CN108298564A (en) | A method of it is crystallized using electrodeposition lean solution production vulcanized sodium | |
| CN208636651U (en) | A kind of preparation facilities of organic developer for negative photoresist |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190625 |
|
| RJ01 | Rejection of invention patent application after publication |