CN105319143A - Method and system for measuring content of calcium stearate in lubricant - Google Patents
Method and system for measuring content of calcium stearate in lubricant Download PDFInfo
- Publication number
- CN105319143A CN105319143A CN201410374261.XA CN201410374261A CN105319143A CN 105319143 A CN105319143 A CN 105319143A CN 201410374261 A CN201410374261 A CN 201410374261A CN 105319143 A CN105319143 A CN 105319143A
- Authority
- CN
- China
- Prior art keywords
- lubricant
- fatty acid
- content
- calcium stearate
- acid
- 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.)
- Granted
Links
- 239000000314 lubricant Substances 0.000 title claims abstract description 82
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 title claims abstract description 56
- 239000008116 calcium stearate Substances 0.000 title claims abstract description 56
- 235000013539 calcium stearate Nutrition 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000002253 acid Substances 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- 238000001035 drying Methods 0.000 claims description 34
- 239000012071 phase Substances 0.000 claims description 34
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 29
- 239000000194 fatty acid Substances 0.000 claims description 29
- 229930195729 fatty acid Natural products 0.000 claims description 29
- 150000004665 fatty acids Chemical class 0.000 claims description 29
- 239000006259 organic additive Substances 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 19
- 238000000605 extraction Methods 0.000 claims description 16
- 235000021588 free fatty acids Nutrition 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 239000008346 aqueous phase Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000003760 magnetic stirring Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000007865 diluting Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 125000003944 tolyl group Chemical group 0.000 claims description 3
- 235000021355 Stearic acid Nutrition 0.000 abstract description 31
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 abstract description 31
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 abstract description 31
- 239000008117 stearic acid Substances 0.000 abstract description 31
- 238000002411 thermogravimetry Methods 0.000 abstract description 17
- 230000004580 weight loss Effects 0.000 abstract description 5
- 125000001931 aliphatic group Chemical group 0.000 abstract 2
- 239000005030 aluminium foil Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000011575 calcium Substances 0.000 description 10
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 10
- 238000005259 measurement Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- CKDDRHZIAZRDBW-UHFFFAOYSA-N henicosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCC(O)=O CKDDRHZIAZRDBW-UHFFFAOYSA-N 0.000 description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 6
- 229910052791 calcium Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 235000021314 Palmitic acid Nutrition 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- 150000004668 long chain fatty acids Chemical class 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 150000007524 organic acids Chemical class 0.000 description 3
- 238000013517 stratification Methods 0.000 description 3
- 238000001757 thermogravimetry curve Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000012749 thinning agent Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
Abstract
The invention discloses a method and system for measuring the content of calcium stearate in a lubricant. The method comprises: extracting aliphatic acid and other organic components contained in the lubricant; measuring the weight loss of aliphatic acid in a temperature range through thermogravimetric analysis; and measuring the content of calcium stearate in the lubricant. According to the method, a thermogravimetric analyzer is adopted for directly measuring the content of stearic acid to calculate the content of calcium stearate. Relevant influence factors are excluded, and therefore, the obtained content of stearic acid is relatively accurate.
Description
Technical field
The present invention relates to lubricant, be specifically related to measuring method and the system of calcium stearate levels in lubricant.
Background technology
Lubricant is the chemical reagent that must add of paper manufacturing systems, but if lubricant quality does not pass a test, can cause cutting knife Fast Wearing, and paper powder increases and increases papermaking cost.Therefore the effective ingredient evaluating lubricant has very important meaning to our production.
Well do not evaluate the method for lubricant effective ingredient at present, in GB, mainly the content of calcium stearate is measured, after analyzing calcium ion content, calculate the content of calcium stearate.In fact and unreliable but if be added into the materials such as calcium carbonate in lubricant, so-called effective ingredient can be caused to increase, therefore this method.
Someone propose with extract admittedly containing and acid value to calculate the method for calcium stearate levels, but its constant concentration can improve by adding polyprotonic acid or polymer substance, to reach the effect improving and calculate content in a lot of bad businessman.Therefore, this method is also unreliable.
Therefore, need to develop a kind of method and system measuring hard fatty acids calcium content in lubricant more reliably.
Summary of the invention
The object of the invention is to set up by using TGA to carry out further analyzing after acidifying, extraction to get rid of because bad businessman adds the higher problem of result that calcium carbonate, polyprotonic acid and polymer substance cause in the lubricant, quantitative test is carried out to the effective ingredient (calcium stearate) of different manufacturers lubricant.
For achieving the above object, according to an aspect of the present invention, provide a kind of method measuring calcium stearate levels in lubricant, it is characterized in that, said method comprising the steps of:
Step one: dilute described lubricant, then uses excess acid to generate free fatty acid to after lubricant acidifying;
Step 2: other organic additive in free fatty acid and lubricant is extracted with organic solvent;
Step 3: the fatty acid in mensuration lubricant and the content of other organic additive;
Step 4: the weightlessness in a temperature range measuring fatty acid; And
Step 5: the content being calculated calcium stearate in described lubricant by fatty acid and the weight of organic additive and the ratio of the weightlessness of described fatty acid in a described temperature range.
Preferably, in step 2, use separating funnel by other organic additive of extracting in the free fatty acid that obtains and lubricant and all the other separating substances.
Preferably, in step 3, only obtain what obtain from step 2 solid and obtained solid is weighed containing free fatty acid carries out drying with the solution of other organic additive, thus obtaining the content of fatty acid and other organic additive.
Preferably, when drying, bake out temperature is set as 103 DEG C to 107 DEG C.Preferably, bake out temperature should meet.
Preferably, in step 4, thermogravimetric analyzer is adopted to measure the weightlessness in a temperature range of fatty acid.
Preferably, acid lubricant being carried out to acidifying is hydrochloric acid, and best, the concentration of described hydrochloric acid is 37%.
Preferably, in step 2, described organic solvent is toluene, and carries out insulated and stirred at least 30 minutes to the mixed solution comprising lubricant, organic solvent and water at a certain temperature, until oil phase and aqueous phase layering, and oil phase present transparent till.
According to a further aspect in the invention, additionally provide a kind of system of the calcium stearate levels measured in lubricant, it is characterized in that, described system comprises:
Air mix facilities, described air mix facilities is used for diluting described lubricant;
Acidizing device, described acidizing device is used for carrying out acidifying to via the lubricant after described air mix facilities dilution, thus generates free fatty acid;
Extraction equipment, described extraction equipment is used for the fatty acid in the lubricant after described acidizing device acidifying and other organic additive to extract;
Drying unit, described drying unit is used for the fatty acid obtained through described extraction equipment and other organic additive to dry;
Weighing device, described weighing device is used for weighing to drying by described drying unit the material obtained; And
Thermogravimetric analyzer, described thermogravimetric analyzer is used for measuring drying through described drying unit the material obtained, and this is determined as the weightlessness of fatty acid in a temperature range measured in described lubricant.
Preferably, described extraction equipment comprises magnetic stirring apparatus and the separating funnel of temperature-controllable, described magnetic stirring apparatus is used for carrying out constant temperature stirring to the lubricant solution after dilution and acidifying, and described separating funnel is used for being separated with aqueous phase the oil phase of the lubricant solution after stirring.
Preferably, described drying unit is baking oven.
The inventive method adopts thermogravimetric analyzer directly to test stearic content to calculate the content of calcium stearate, and the stearic acid content value obtained eliminates relevant influence factor, therefore relatively accurate.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the method for stearic acid content in the measurement lubricant according to one embodiment of the invention;
Fig. 2 is the block diagram of the system of stearic acid content in the measurement lubricant according to one embodiment of the invention;
Fig. 3 is the calcium stearate thermal gravimetric analysis curve figure of the embodiment one of stearic acid content in measurement lubricant of the present invention;
Fig. 4 is the calcium stearate thermal gravimetric analysis curve figure of the embodiment two of stearic acid content in measurement lubricant of the present invention; And
Fig. 5 is the calcium stearate thermal gravimetric analysis curve figure of the embodiment three of stearic acid content in measurement lubricant of the present invention.
Embodiment
Below with reference to accompanying drawing, preferred embodiment of the present invention is described in detail, so that clearer understanding objects, features and advantages of the present invention.It should be understood that embodiment shown in the drawings is not limitation of the scope of the invention, and the connotation just in order to technical solution of the present invention is described.In accompanying drawing, the same or analogous Reference numeral of identical element indicates.
Terminological interpretation:
Thermogravimetric analysis (ThermogravimetricAnalysis, TG or TGA): a kind of thermoanalysis technology referring to quality and the temperature variation relation measuring testing sample under programed temperature, is used for the thermal stability of research material and component.TGA is the detection means relatively commonly used in research and development and quality control.Thermogravimetric analysis in the material analysis of reality often and other analytical approachs be used in conjunction, carry out Thermal Synthetic Analysis, comprehensive accurate analysis material.
As shown in Figure 1, according to the method ultimate principle of stearic acid content in the measurement lubricant of one embodiment of the invention for the fatty acid comprised in lubricant and other organic moiety are extracted, and measure the weightlessness of fatty acid in a temperature range by thermogravimetry, and then measure the calcium stearate levels in lubricant.Particularly, said method comprising the steps of:
Step one: use the thinning agents such as water to dilute lubricant to be measured, then uses excess acid to generating free fatty acid after lubricant acidifying;
Step 2: other organic additive in free fatty acid and lubricant is extracted with organic solvent;
Step 3: the fatty acid in mensuration lubricant and the content of other organic additive;
Step 4: the weightlessness in a temperature range measuring fatty acid; And
Step 5: the content being calculated calcium stearate in described lubricant by the ratio of the weightlessness in the weight of fatty acid and organic additive and a described temperature range.
In step one, preferably, thinning agent is water.Preferably, the acid carrying out acidifying to lubricant is the concentration of concentrated hydrochloric acid (HCl) described hydrochloric acid is 35% to 37%.Preferably, the concentration of described hydrochloric acid is about 37%.Here, adding hydrochloric acid is that reaction equation is as follows: Ca (C in order to make calcium stearate acidolysis be stearic acid and lime chloride
17h
36cOO)
2+ 2HCL=CaCL
2+ 2C
17h
35cOOH.
In step 2, preferably, use separating funnel by other organic additive of extracting in the free fatty acid that obtains and lubricant and all the other separating substances.Preferably, described organic solvent is toluene, and wherein adding toluene is the stearic acid obtained to extract acidolysis.Preferably, at a certain temperature, insulated and stirred is carried out at least 30 minutes to the mixed solution comprising lubricant, organic solvent and water, until oil phase and aqueous phase layering, and oil phase present transparent till.Preferably, described whipping temp is selected from the arbitrary temperature value between 20 DEG C to 30 DEG C.Herein, oil phase is mainly stearic acid, or is added into other long-chain fatty acid by supplier, as hexadecanoic acid, Heptadecanoic acide or heneicosanoic acid etc.
In step 3, only obtain what obtain from step 2 solid and obtained solid is weighed containing free fatty acid carries out drying with the solution of other organic additive, thus obtaining the content of fatty acid and other organic additive.Preferably, dried by baking box.Preferably, when drying, bake out temperature is set as 103 degree to 105 degree.Preferably, weighed by balance.
In step 4, thermogravimetric analyzer is adopted to measure the weightlessness in a temperature range of fatty acid.Wherein thermogravimetric analyzer (ThermoGravimetricAnalyzer) is a kind of instrument utilizing thermogravimetry (TG) detection material temperature-mass change relation.Thermogravimetry (TG) is under temperature programmed control, and the quality of measurement of species is with the variation relation of temperature (or time).
Preferably, this thermogravimetric analyzer is in inert atmosphere (such as N
2) in, sample to be analyzed (solid matter after extraction after upper oil phase oven dry) is in thermogravimetric analyzer ramped heating schedule process, to volatilize gradually decomposition, the quality of the precision balance automatic real-time monitoring sample of instrument internal, according to the weight loss in stearic decomposition temperature (120-350 degree) scope, obtain stearic acid content in sample.
When thermogravimetric analyzer operates, sample (about 5-10mg) is placed in the alchlor crucible (70ul) that thermogravimetric analyzer is special, instrument automatic weighing sample quality, automatically after entering sample bin, according to the program (N2flowrate:50ml/min of method setting in workstation; Oventemperature:25 DEG C-500 DEG C; Rate:10 DEG C/min).
By above-mentioned measuring method, bad businessman can be avoided to improve the measured value of the calcium stearate in lubricant by interpolation organic acid or calcium.Therefore, this method can measure the content of the actual calcium stearate in lubricant relatively accurately.
Fig. 2 illustrates the system 100 according to a kind of calcium stearate levels measured in lubricant of the present invention.As shown in Figure 2, described system 100 comprises: air mix facilities 1, and described air mix facilities 1 is for diluting described lubricant; Acidizing device 2, described acidizing device 2 for carrying out acidifying to via the lubricant after described air mix facilities 1 dilution, thus generates free fatty acid; Extraction equipment 3, described extraction equipment 3 is for extracting the fatty acid in the lubricant after the acidifying of described acidizing device 2 and other organic additive; Drying unit 4, described drying unit 4 is dried with other organic additive for the fatty acid will obtained through described extraction equipment 3; Weighing device 5, described weighing device 5 is for weighing to drying by described drying unit 4 material obtained; And thermogravimetric analyzer 6, described thermogravimetric analyzer 6 is for measuring drying through described drying unit 4 material obtained, and this is determined as the weightlessness of fatty acid in a temperature range measured in described lubricant.
Preferably, described air mix facilities 1 and described acidizing device 2 are same device, such as, for be made up of conical flask and graduated cylinder (not shown).In use, lubricant is contained in conical flask, and water and acid to be added in conical flask respectively by different graduated cylinders thus realize dilution and acidifying.
Preferably, above-mentioned extraction equipment comprises magnetic stirring apparatus and the separating funnel of temperature-controllable, described magnetic stirring apparatus is used for carrying out constant temperature stirring to the lubricant solution after dilution and acidifying, and described separating funnel is used for being separated with aqueous phase the oil phase of the lubricant solution after stirring.But, it will be understood by those skilled in the art that above-mentioned extraction equipment also can be any suitable device being suitable for extracting.And extraction equipment can be independent device, or be integrated in whole measuring system.
Preferably, described drying unit is baking oven, extracts the oil phase substance obtained and is placed in baking oven, toast certain hour at a certain temperature and become solid-state.But it will be understood by those skilled in the art that drying unit can be to heat oil phase substance at a certain temperature, make it become solid-state heating arrangement, it can be integrated in system, also can exist as independent device.
Thermogravimetric analyzer can select any suitable thermogravimetric analyzer known in the art.
Embodiment 1
In 250ml conical flask, with a certain model lubricant that the A company that electronic balance accurately takes about 10g (W) produces, add the water (such as using graduated cylinder) of 40ml, dilute it, add HCl concentrated hydrochloric acid (concentration 37%) 5ml (use pipettor), and in stirring at normal temperature 5 minutes, then add the toluene (such as using graduated cylinder) of 50ml, as the stearic solvent of dissolving.Conical flask is airtight and be positioned on the heating magnetite stirrer of temp. controllable, and temperature is set in 60 DEG C, insulated and stirred at least 30 minutes, to oil phase and aqueous phase layering, and oil phase present transparent till.
Pipette upper oil phase 5ml with pipettor and be placed in 105 degree of baking ovens, dry 4h (upper oil phase is mainly stearic acid, or is added into other long-chain fatty acid by supplier, as hexadecanoic acid, Heptadecanoic acide or heneicosanoic acid etc.).
The solid matter obtained after oven dry, carries out thermogravimetric analysis, obtains stearic content according to the stearic weightless temperature scope (120-350 degree) on thermogravimetric curve.
The content of calcium stearate is drawn by following formula:
Calcium stearate %=X
1* S%*50/w/607.02/568.96 (1)
In formula (1): X
1for the stearic content obtained by the percent weight loss within the scope of 120-350 degree on TG curve; 607.02 be the molecular weight of calcium stearate; 568.96 is 2 moles of stearic molecular weight.S% is obtained by following formulae discovery
Wherein:
W
2: the aluminium foil weight after drying
W
0: aluminium foil weight
W
1: example weight
Be 33.93% by the calcium stearate levels of A company this batch of lubricant of said method step measurements.
Comparative example 1
By solid content and stearic acid content COMPREHENSIVE CALCULATING calcium stearate levels
1) in 250ml conical flask, the A company of about 10g (W) is accurately taken with a collection of lubricant, add the water of 40ml, dilute it, add the toluene of 50g again, as the stearic solvent of dissolving, magnetic stirring apparatus stirs, adds HCl concentrated hydrochloric acid (concentration 37%) 5ml, and in stirring at normal temperature 5 minutes.Conical flask is airtight and be positioned on the heating magnetite stirrer of temp. controllable, and start to heat up, temperature is set in 60 DEG C, insulated and stirred at least 30 minutes, to oil phase and aqueous phase layering, and oil phase present transparent till.(this process is: adding hydrochloric acid is that reaction equation is as follows: Ca (C in order to make calcium stearate acidolysis be stearic acid and lime chloride
17h
36cOO)
2+ 2HCL=CaCL
2+ 2C
17h
35cOOH, adding toluene is the stearic acid obtained to extract acidolysis.)
2) stratification, get oil reservoir (upper strata), test its acid value:
Wherein,
The N of N:KOH
The milliliter number (ml) of V:KOH institute titration
W: the weight (g) of sample
3) get upper strata oil reservoir 3g and be placed in 105 degree of baking ovens, dry 4h, the solid content of test oil reservoir;
W
2: the aluminium foil weight after drying, W
0: aluminium foil weight, W
1: example weight
4) calcium stearate levels is calculated by solid content, acid value, stearic acid content
Calcium stearate %=50/W × AV × 38 ÷ 56.11 ÷ 2000+50/W*S
Wherein X
1for the acid value of upper oil phase, W is sample size.
The calcium stearate levels of this model of A company measured by the method for comparative example 1 is 41.59%.
Embodiment 2
In 250ml conical flask, with a certain model lubricant that the B company that electronic balance accurately takes about 10g (W) produces, add the water (such as using graduated cylinder) of 40ml, dilute it, add HCl concentrated hydrochloric acid (concentration 37%) 5ml (use pipettor), and in stirring at normal temperature 5 minutes, then add the toluene (such as using graduated cylinder) of 50ml, as the stearic solvent of dissolving.Conical flask is airtight and be positioned on the heating magnetite stirrer of temp. controllable, and temperature is set in 60 DEG C, insulated and stirred at least 30 minutes, to oil phase and aqueous phase layering, and oil phase present transparent till.
Pipette upper oil phase 5ml with pipettor and be placed in 105 degree of baking ovens, dry 4h (upper oil phase is mainly stearic acid, or is added into other long-chain fatty acid by supplier, as hexadecanoic acid, Heptadecanoic acide or heneicosanoic acid etc.).
The solid matter obtained after oven dry, carries out thermogravimetric analysis, obtains stearic content according to the stearic weightless temperature scope (120-350 degree) on thermogravimetric curve.
The content of calcium stearate is drawn by following formula:
Calcium stearate %=X
1* S%*50/w/607.02/568.96 (1)
In formula (1): X
1for the stearic content obtained by the percent weight loss within the scope of 120-350 degree on TG curve; 607.02 be the molecular weight of calcium stearate; 568.96 is 2 moles of stearic molecular weight.S% is obtained by following formulae discovery
Wherein:
W
2: the aluminium foil weight after drying
W
0: aluminium foil weight
W
1: example weight
Be 29.20% by the calcium stearate levels of A company this batch of lubricant of said method step measurements.
Comparative example 2
By solid content and stearic acid content COMPREHENSIVE CALCULATING calcium stearate levels
2) in 250ml conical flask, the B company of about 10g (W) is accurately taken with a collection of lubricant, add the water of 40ml, dilute it, add the toluene of 50g again, as the stearic solvent of dissolving, magnetic stirring apparatus stirs, adds HCl concentrated hydrochloric acid (concentration 37%) 5ml, and in stirring at normal temperature 5 minutes.Conical flask is airtight and be positioned on the heating magnetite stirrer of temp. controllable, and start to heat up, temperature is set in 60 DEG C, insulated and stirred at least 30 minutes, to oil phase and aqueous phase layering, and oil phase present transparent till.(this process is: adding hydrochloric acid is that reaction equation is as follows: Ca (C in order to make calcium stearate acidolysis be stearic acid and lime chloride
17h
36cOO)
2+ 2HCL=CaCL
2+ 2C
17h
35cOOH, adding toluene is the stearic acid obtained to extract acidolysis.)
2) stratification, get oil reservoir (upper strata), test its acid value:
Wherein,
The N of N:KOH
The milliliter number (ml) of V:KOH institute titration
W: the weight (g) of sample
4) get upper strata oil reservoir 3g and be placed in 105 degree of baking ovens, dry 4h, the solid content of test oil reservoir;
W
2: the aluminium foil weight after drying, W
0: aluminium foil weight, W
1: example weight
4) calcium stearate levels is calculated by solid content, acid value, stearic acid content
Calcium stearate %=50/W × AV × 38 ÷ 56.11 ÷ 2000+50/W*S
Wherein X
1for the acid value of upper oil phase, W is sample size.
The calcium stearate levels of this model of A company measured by the method for comparative example 1 is 34.16%.
Embodiment 3
In 250ml conical flask, with a certain model lubricant that the C company that electronic balance accurately takes about 10g (W) produces, add the water (such as using graduated cylinder) of 40ml, dilute it, add HCl concentrated hydrochloric acid (concentration 37%) 5ml (use pipettor), and in stirring at normal temperature 5 minutes, then add the toluene (such as using graduated cylinder) of 50ml, as the stearic solvent of dissolving.Conical flask is airtight and be positioned on the heating magnetite stirrer of temp. controllable, and temperature is set in 60 DEG C, insulated and stirred at least 30 minutes, to oil phase and aqueous phase layering, and oil phase present transparent till.
Pipette upper oil phase 5ml with pipettor and be placed in 105 degree of baking ovens, dry 4h (upper oil phase is mainly stearic acid, or is added into other long-chain fatty acid by supplier, as hexadecanoic acid, Heptadecanoic acide or heneicosanoic acid etc.).
The solid matter obtained after oven dry, carries out thermogravimetric analysis, obtains stearic content according to the stearic weightless temperature scope (120-350 degree) on thermogravimetric curve.
The content of calcium stearate is drawn by following formula:
Calcium stearate %=X
1* S%*50/w/607.02/568.96 (1)
In formula (1): X
1for the stearic content obtained by the percent weight loss within the scope of 120-350 degree on TG curve; 607.02 be the molecular weight of calcium stearate; 568.96 is 2 moles of stearic molecular weight.S% is obtained by following formulae discovery
Wherein:
W
2: the aluminium foil weight after drying
W
0: aluminium foil weight
W
1: example weight
Be 12.44% by the calcium stearate levels of A company this batch of lubricant of said method step measurements.
Comparative example 3
By solid content and stearic acid content COMPREHENSIVE CALCULATING calcium stearate levels
3) in 250ml conical flask, the C company of about 10g (W) is accurately taken with a collection of lubricant, add the water of 40ml, dilute it, add the toluene of 50g again, as the stearic solvent of dissolving, magnetic stirring apparatus stirs, adds HCl concentrated hydrochloric acid (concentration 37%) 5ml, and in stirring at normal temperature 5 minutes.Conical flask is airtight and be positioned on the heating magnetite stirrer of temp. controllable, and start to heat up, temperature is set in 60 DEG C, insulated and stirred at least 30 minutes, to oil phase and aqueous phase layering, and oil phase present transparent till.(this process is: adding hydrochloric acid is that reaction equation is as follows: Ca (C in order to make calcium stearate acidolysis be stearic acid and lime chloride
17h
36cOO)
2+ 2HCL=CaCL
2+ 2C
17h
35cOOH, adding toluene is the stearic acid obtained to extract acidolysis.)
2) stratification, get oil reservoir (upper strata), test its acid value:
Wherein,
The N of N:KOH
The milliliter number (ml) of V:KOH institute titration
W: the weight (g) of sample
5) get upper strata oil reservoir 3g and be placed in 105 degree of baking ovens, dry 4h, the solid content of test oil reservoir;
W
2: the aluminium foil weight after drying, W
0: aluminium foil weight, W
1: example weight
4) calcium stearate levels is calculated by solid content, acid value, stearic acid content
Calcium stearate %=50/W × AV × 38 ÷ 56.11 ÷ 2000+50/W*S
Wherein X
1for the acid value of upper oil phase, W is sample size.
The calcium stearate levels of this model of A company measured by the method for comparative example 1 is 34.65%.
As can be seen from above three embodiments, for the lubricant product of different company, adopt method of testing measured result of the present invention all on the low side than the existing method of tradition, reason is that existing method is all the content being calculated calcium stearate by the stearic acid in working sample or calcium content, therefore some company can according to these indirectly assay method add other organic acids (as add palmitic acid, adopt titrimetry by Simultaneously test when measuring stearic acid, thus increase institute and survey stearic content) or interpolation calcium (as interpolation calcium carbonate etc., detected when measuring calcium content simultaneously, thus increase survey the content of calcium), the content of the calcium stearate that existing method is recorded is higher.As can be seen from the thermogravimetric analysis spectrogram of three examples, three companies all add organic acid content, wherein add at most with example 3.This is meaning of the present invention.In contrast, the inventive method then adopts thermogravimetric analyzer directly to test stearic content to calculate the content of calcium stearate, and the stearic acid content value obtained eliminates relevant influence factor, therefore relatively accurate.
Below described preferred embodiment of the present invention in detail, but it will be appreciated that, after having read above-mentioned instruction content of the present invention, those skilled in the art can make various changes or modifications the present invention.These equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. measure a method for calcium stearate levels in lubricant, it is characterized in that, said method comprising the steps of:
Step one: dilute described lubricant, then uses excess acid to generate free fatty acid to after lubricant acidifying;
Step 2: other organic additive in free fatty acid and lubricant is extracted with organic solvent;
Step 3: the fatty acid in mensuration lubricant and the content of other organic additive;
Step 4: the weightlessness in a temperature range measuring fatty acid; And
Step 5: the content being calculated calcium stearate in described lubricant by fatty acid and the weight of organic additive and the ratio of the weightlessness of described fatty acid in a described temperature range.
2. method according to claim 1, is characterized in that, in step 2, uses separating funnel by other organic additive of extracting in the free fatty acid that obtains and lubricant and all the other separating substances.
3. method according to claim 1, it is characterized in that, in step 3, only obtain what obtain from step 2 solid and obtained solid is weighed containing free fatty acid carries out drying with the solution of other organic additive, thus obtaining the content of fatty acid and other organic additive.
4. method according to claim 3, is characterized in that, when drying, bake out temperature is set as 103 DEG C to 107 DEG C.
5. method according to claim 1, is characterized in that, in step 4, adopts thermogravimetric analyzer to measure the weightlessness in a temperature range of fatty acid.
6. method according to claim 1, is characterized in that, described acid is 35% hydrochloric acid.
7. method according to claim 1, it is characterized in that, in step 2, described organic solvent is toluene, and at a certain temperature insulated and stirred is carried out at least 30 minutes to the mixed solution comprising lubricant, organic solvent and water, until oil phase and aqueous phase layering, and oil phase present transparent till.
8. measure a system for the calcium stearate levels in lubricant, it is characterized in that, described system comprises:
Air mix facilities, described air mix facilities is used for diluting described lubricant;
Acidizing device, described acidizing device is used for carrying out acidifying to via the lubricant after described air mix facilities dilution, thus generates free fatty acid;
Extraction equipment, described extraction equipment is used for the fatty acid in the lubricant after described acidizing device acidifying and other organic additive to extract;
Drying unit, described drying unit is used for the fatty acid obtained through described extraction equipment and other organic additive to dry;
Weighing device, described weighing device is used for weighing to drying by described drying unit the material obtained; And
Thermogravimetric analyzer, described thermogravimetric analyzer is used for measuring drying through described drying unit the material obtained, and this is determined as the weightlessness of fatty acid in a temperature range measured in described lubricant.
9. system according to claim 8, it is characterized in that, described extraction equipment comprises magnetic stirring apparatus and the separating funnel of temperature-controllable, described magnetic stirring apparatus is used for carrying out constant temperature stirring to the lubricant solution after dilution and acidifying, and described separating funnel is used for being separated with aqueous phase the oil phase of the lubricant solution after stirring.
10. system according to claim 8, is characterized in that, described drying unit is baking oven.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410374261.XA CN105319143B (en) | 2014-07-31 | 2014-07-31 | Measure the method and system of calcium stearate levels in lubricant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410374261.XA CN105319143B (en) | 2014-07-31 | 2014-07-31 | Measure the method and system of calcium stearate levels in lubricant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105319143A true CN105319143A (en) | 2016-02-10 |
| CN105319143B CN105319143B (en) | 2018-11-16 |
Family
ID=55247009
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410374261.XA Active CN105319143B (en) | 2014-07-31 | 2014-07-31 | Measure the method and system of calcium stearate levels in lubricant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105319143B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770420A (en) * | 2016-11-18 | 2017-05-31 | 中国石油天然气股份有限公司 | A kind of rock pyrolysis analysis method containing siderite deposit |
| CN112945793A (en) * | 2021-03-30 | 2021-06-11 | 福建中烟工业有限责任公司 | Method and device for detecting content of liquid content in carrier gel |
| CN114354840A (en) * | 2022-01-10 | 2022-04-15 | 广东鑫达新材料科技有限公司 | Analysis method for components and content of lubricant in composite stabilizer |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204101403U (en) * | 2014-07-31 | 2015-01-14 | 芬欧汇川(中国)有限公司 | Measure the system of calcium stearate levels in lubricant |
-
2014
- 2014-07-31 CN CN201410374261.XA patent/CN105319143B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204101403U (en) * | 2014-07-31 | 2015-01-14 | 芬欧汇川(中国)有限公司 | Measure the system of calcium stearate levels in lubricant |
Non-Patent Citations (2)
| Title |
|---|
| ANA PAULA D. MOREIRA ET AL.: "Monitoring of calcium stearate formation by thermogravimetry", 《J THERM ANAL CALORIM》 * |
| 冯练享等: "高固含量硬脂酸钙润滑剂的研制", 《西南造纸》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770420A (en) * | 2016-11-18 | 2017-05-31 | 中国石油天然气股份有限公司 | A kind of rock pyrolysis analysis method containing siderite deposit |
| CN112945793A (en) * | 2021-03-30 | 2021-06-11 | 福建中烟工业有限责任公司 | Method and device for detecting content of liquid content in carrier gel |
| CN114354840A (en) * | 2022-01-10 | 2022-04-15 | 广东鑫达新材料科技有限公司 | Analysis method for components and content of lubricant in composite stabilizer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105319143B (en) | 2018-11-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103424443B (en) | A kind of ion selecting electrode determining method of Oil repellent in grain, Vegetables and fruits | |
| CN105319143A (en) | Method and system for measuring content of calcium stearate in lubricant | |
| CN108414675B (en) | Method for rapidly determining low-concentration boric acid in aqueous solution by using pH meter | |
| CN106153498A (en) | A kind of new method detecting solute concentration in solution and device thereof | |
| CN106093098A (en) | A kind of measure the method for copper content in fireworks and firecrackers firework medicament | |
| CN204214880U (en) | A kind of microcomputer pH value instrument | |
| CN103293175A (en) | Method for measuring chemical components of liquid sodium silicate | |
| CN101949877A (en) | Method for measuring edible oleic acid value based on conductivity | |
| CN204101403U (en) | Measure the system of calcium stearate levels in lubricant | |
| CN101303304B (en) | Method for testing acrylic amide in food | |
| CN106950215B (en) | A kind of method of sodium carbonate or sodium bicarbonate content in measurement solid sample | |
| CN106248709A (en) | A kind of measure the method for potassium content in fireworks and firecrackers firework medicament | |
| CN106168587A (en) | A kind of measure the method for iron content in fireworks and firecrackers firework medicament | |
| CN106124546A (en) | A kind of measure the method for potassium content in industry potassium chlorate | |
| CN106324005A (en) | Method for determining content of Ba in pyrotechnic composition for fireworks and firecrackers | |
| CN106093097A (en) | A kind of measure the method for content of strontium in fireworks and firecrackers firework medicament | |
| CN106370685A (en) | Method for determining content of potassium in industrial potassium chloride | |
| CN107179339A (en) | It is a kind of at the same determine zinc electrolyte in copper cadmium nickel cobalt content method | |
| CN106908509A (en) | The quick and quantitative detecting method of doping paraffin in a kind of lard | |
| CN106168586A (en) | A kind of measure the method for iron content in fireworks and firecrackers iron powder | |
| CN105954262A (en) | {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery | |
| CN109283165A (en) | The preparation method and application of water microanalysis fluorescent test paper strip in a kind of organic reagent | |
| CN106370686A (en) | Method for determining copper content in basic copper carbonate for fireworks and firecrackers | |
| CN110849854A (en) | Hg determination by BA-Eu-MOF composite material2+And CH3Hg+Method of content | |
| CN106290437A (en) | A kind of measure the method for iron content in fireworks and firecrackers ferroso-ferric oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |