CN109991261A - The measurement device and measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point - Google Patents
The measurement device and measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point Download PDFInfo
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- CN109991261A CN109991261A CN201711470370.1A CN201711470370A CN109991261A CN 109991261 A CN109991261 A CN 109991261A CN 201711470370 A CN201711470370 A CN 201711470370A CN 109991261 A CN109991261 A CN 109991261A
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- congealing point
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- airshower
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000005259 measurement Methods 0.000 title claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052753 mercury Inorganic materials 0.000 claims abstract description 21
- 239000012530 fluid Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000001304 sample melting Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims description 12
- 238000007598 dipping method Methods 0.000 claims description 5
- 230000010076 replication Effects 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000001993 wax Substances 0.000 description 37
- 229940099259 vaseline Drugs 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000001828 Gelatine Substances 0.000 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- -1 weaving Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/04—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of melting point; of freezing point; of softening point
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The measurement device and measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point, measurement device includes: congealing point thermometer, transparent airshower, rotating device and heating device, there is plug on transparent airshower, congealing point thermometer is mounted on the central axis of plug, rotating device is provided with support base, heating device is used for heating transparent airshower, and wherein heating device is heat gun or infrared heater.Measuring method includes: by sample melting for liquid；Sample is dipped using congealing point thermometer；Congealing point thermometer with fluid sample is installed on transparent airshower；The transparent airshower rotated on rotating device is heated, heating intensity is controlled, stops heating after thermometer reaches predetermined temperature, observe the waxy and temperature reading on mercury ball, when the waxy rotation with thermometer mercury ball, temperature value, the as congealing point of the sample are read immediately.The device of the invention is at low cost, simple to operate, and result precision is high.
Description
Technical field
The invention belongs to sample congealing point testing fields, and in particular to the measurement dress of a kind of Fischer-Tropsch wax and pertroleum wax congealing point
It sets and measuring method.
Background technique
The sample of cooling fusing stops the freezing point that the temperature of flowing is sample under the defined conditions.Fischer-Tropsch wax and stone
At this temperature, solid-state may be presented or close to solid-state or semi-solid state, the constituent of this and tested sample in oily wax
It is related.If vaseline, congealing point is related with the gelatine structure form of sample while cooling.It is that indirect reaction wax class product is average
One index of molecular size range and purity and at normal temperature soft or hard degree, can react storage, processing, transport safety with
Difficulty or ease.Domestic special wax research and development lay particular stress on concern fusing point, dropping point and drip melt especially using Fischer-Tropsch wax as the research and development of raw material
Point, and external special wax manufacturer and user is interested, more pay attention to is this index of congealing point.With South Africa Sha Suowei generation
Table, the series such as hot melt adhesive, ink/coating, plastics, rubber, light wax, weaving, wax crayon, candle, beauty and make-up special wax is almost
Congealing point is all included in important indicator, at home, existing Shanxi enterprise, can be pre- using congealing point as its product code numbering
Phase from now on will certainly gradually realize special wax people the importance of congealing point, have more and more production firms solidifying
Important quality index one of of the solid point as its product.
There is manual operations inconvenience in the prior art, be skilled in technique to operative employee and require height, and what completion analysis test needed sets
It is specific as follows for the disadvantages of more, equipment investment is larger, analysis time is longer:
1, equipment investment expense is larger, in addition to needing to buy congealing point thermometer, conical flask and speed regulation rotating machinery, also
Constant temperature oven is needed to configure, and it is big to account for experimental bench area, about needs to occupy nearly 2 meters of long experimental benches；
2, actual operation there are steps more, long flow path, spends the time long, and overall process is outer except preparing, main including 6 mistakes
Journey, total time-consuming need 2 hours or so according to sample difference；
3, the bad assurance of operating condition protects both hands with towel or gloves, is easy scald, and operation difficulty is very big.
Summary of the invention
To be solved by this invention is simplified Fischer-Tropsch wax and pertroleum wax includes that its fraction and residual wax (including vaseline) freeze
Condensation point analyzes operating process, shortens analysis time, finds and a kind of more safe and simple, easily operated fast and accurately congeals
Point analysis method.
The measurement device of Fischer-Tropsch wax and pertroleum wax congealing point of the invention includes: congealing point thermometer, transparent air bath dress
It sets, rotating device and heating device, wherein having plug on transparent airshower, the outer of plug is provided with air slot, congeals
Point thermometer is mounted on the central axis of plug, and support base, the transparent air are provided on the horizontal rotating shaft of rotating device
Bath apparatus is fixed on the support base, and heating device is used for heating transparent airshower, and heating device is heat gun or red
Outside line heater.The transparent airshower can be the containers such as flask.
Preferably, the rotating device is small-sized speed regulating motor.
Preferably, the symmetrical overlapping of axles in the axle center of the horizontal rotating shaft and transparent airshower.
Preferably, the mercury ball bottom of the congealing point thermometer is to transparent airshower bottom about 10~15mm.
Preferably, the transparent airshower is scheduled on the support base by the way that magnetic sheet is same.
The measuring method of Fischer-Tropsch wax and pertroleum wax congealing point of the invention includes:
(1) by sample melting for liquid；
(2) sample is dipped using congealing point thermometer；
(3) the congealing point thermometer with fluid sample is installed on transparent airshower；
(4) the transparent airshower rotated on rotating device is heated, heating intensity is controlled, when thermometer reaches regulation
Stop heating after temperature, observe the waxy and temperature reading on mercury ball, when the waxy rotation with thermometer mercury ball, immediately
Read temperature value, the as congealing point of the sample.
Preferably, by sample melting to be sufficiently stirred after liquid.
Preferably, when dipping sample, fluid sample is made to be sticked to the mercury bulb of thermometer.
Preferably, the revolving speed of the rotating device is 2~3s/ circle.
Preferably, same sample carries out replication, takes the average value of 2-3 measured value congealing as institute's test specimens
Point.
Compared with prior art, the invention has the following advantages:
1, heating equipment can use closed electric furnace and heat gun, and price small in size is low, due to the ingehious design of mode of operation, drop
The low requirement to equipment performance, reduces more than half equipment purchase cost and experimental bench area occupied；
2, process is simplified, analysis testing efficiency is improved, sample, component installation and warm will be dipped in and organically combined, adopted
With first dipping in, sample, arrangement is finally heated to reach the purpose of convenient, safe again.Preparation including sample, time used in overall process
It can be shorten to 0.5 hour or so by 1.5 hours；
3, easy to operate, the i.e. controllable heating rate of heating intensity of heat gun or infrared heater need to be only controlled, is held
Easily reach temperature requirement；
4, result precision is high, and the repeatability and reproducibility of Fischer-Tropsch wax arrives separately at≤0.5 DEG C and≤1.5 DEG C；Residual wax
The repeatability and reproducibility of (including vaseline) arrives separately at≤1 DEG C and≤2.5 DEG C.
Detailed description of the invention
Fig. 1 is the measurement device in the embodiment of the present invention；
Fig. 2 is the flow chart of measuring method of the invention.
1- congealing point thermometer；2- flask；3- rotating device；4- heating device；5- plug；6- flask support base；7- magnetic
Piece.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
In embodiments of the present invention, Fischer-Tropsch wax sample with closed electric furnace heated into fusing and with the mercury ball position of thermometer
Fischer-Tropsch wax drop is dipped, is attached to one as on the conical flask of collet, then be horizontally arranged on rotating machinery, heats flask,
The Fischer-Tropsch wax being sticked on mercury ball is melted, it is cooling until condensation, when Fischer-Tropsch wax drop stops flowing, observation with specified speed
To temperature be exactly freezing point.The present invention is suitable for the test of Fischer-Tropsch wax pour point, including pertroleum wax, vaseline.
As shown in Figure 1, the measurement device of Fischer-Tropsch wax and pertroleum wax congealing point of the invention includes: congealing point thermometer 1, burns
Bottle 2, rotating device 3 and heating device 4 wherein have plug 5 on flask, the outer of plug 5 is provided with air slot, congealing point temperature
Meter is mounted on the central axis of plug, flask support base 6 is provided on the horizontal rotating shaft of rotating device, flask 2 is fixed on burning
On bottle support base 6, heating device 4 is for heating flask 2.Heating device 4 can be for heat gun or infrared heater etc., can be with
Heating is oriented to flask 2.
Rotating device 3 can be small-sized speed regulating motor, 2~3s/ of adjustable speed circle, the axle center of horizontal rotating shaft and flask it is symmetrical
Overlapping of axles.
Transparent airshower of the flask 2 as thermometer can be conical flask, and volume can be 125mL.
The mercury ball bottom of congealing point thermometer 1 is to drag about 10~15mm.
The connection of flask 2 and rotating device 3, can be various ways.Such as it can be magnetic connection, it may be assumed that use heat-resistant adhesive
The magnetic sheet 7 of thick 2-3mm diameter 20-30mm is sticked to drag, magnetic force is recycled to be fixed on the flask of rotating device concentric shafts
On support base.Certainly, in addition to this mode, it can also be that other way is fixedly connected.
As shown in Fig. 2, the measuring method of Fischer-Tropsch wax and pertroleum wax congealing point of the invention includes:
(1) by sample melting for liquid；
(2) sample is dipped using congealing point thermometer；
(3) the congealing point thermometer with fluid sample is installed on flask；
(4) flask rotated on rotating device is heated, heating intensity is controlled, stops after thermometer reaches predetermined temperature
The waxy and temperature reading on mercury ball is observed in heating, when the waxy rotation with thermometer mercury ball, reads temperature immediately
Value, the as congealing point of the sample.
By sample melting to be sufficiently stirred after liquid.
When dipping sample, fluid sample is made to be sticked to the mercury bulb of thermometer.
The revolving speed of rotating device is 2~3s/ circle.
Same sample carries out replication, takes the average value of 2-3 measured value as the congealing point of institute's test specimens.
Embodiment 1
(1) thermometer is mounted on plug central axis, makes thermometer mercury ball bottom to conical flask bottom about 10
~15mm.
(2) sample for taking 50g representative is put into 100ml glass beaker, is heated to 11 DEG C of estimated congealing point or more
(attention is sufficiently stirred).
(3) a drop sample is dipped with the thermometer installed on plug, temperature levels is held and slowly turn several circles, make sample
Even solidification is on mercury ball, then is horizontally mounted on conical flask.
(4) small-sized governor switch is pressed, 2~3s/ of revolving speed circle is adjusted, conical flask is heated with heat gun, until temperature
The groove that meter mercury reaches 99 ± 3 DEG C no longer rises.Heat gun is removed, the drop on mercury ball is observed, when drop is with temperature
When degree meter mercury ball rotation, the temperature of thermometer is read immediately, is accurate to 0.5 DEG C, and record this measured value.Use same sample
Replication is carried out, takes the average value of measured value twice as the congealing point of institute's test specimens.
In measurement, it can recorde the average value of multiple test values, as freezing point, be accurate to 0.25 DEG C.
It is as follows to measure precision requirement:
Repeatability: same operator uses same device, final to same sample test resulting under conditions of constant
As a result deviation, it is desirable that as follows:
Fischer-Tropsch wax (including paraffin distillate)≤0.5 DEG C；Residual wax (including vaseline)≤1.0 DEG C.
Reproducibility: different experiments room, different operation person are mutually indepedent to finally obtained two of same sample test
Result deviation, it is desirable that it is as follows:
Fischer-Tropsch wax (including paraffin distillate)≤1.5 DEG C；Residual wax (including vaseline)≤2.5 DEG C.
The present invention uses cold mounting technique, after dipping appropriate amount of sample with thermometer, installs component at room temperature, instead of
Mounting means after conical flask is preheating to 99 DEG C.Sample heating uses rotary heating technology, at the uniform velocity rotates in test suite
In the case where, it is reduced from conical flask external heat instead of the heating method with constant temperature oven with heat gun or infrared heater
Equipment cost, simplifies operating process.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (10)
1. the measurement device of a kind of Fischer-Tropsch wax and pertroleum wax congealing point, comprising: congealing point thermometer, turns transparent airshower
Dynamic device and heating device, wherein having plug on the transparent airshower, the outer of the plug is provided with air slot, institute
It states congealing point thermometer to be mounted on the central axis of the plug, support is provided on the horizontal rotating shaft of the rotating device
Seat, the transparent airshower are fixed on the support base, and the heating device is for heating the transparent air bath dress
It sets, the heating device is heat gun or infrared heater.
2. measurement device as described in claim 1, which is characterized in that the rotating device is small-sized speed regulating motor.
3. measurement device as described in claim 1, which is characterized in that the axle center of the horizontal rotating shaft and transparent airshower
Symmetrical overlapping of axles.
4. measurement device as described in claim 1, which is characterized in that the mercury ball bottom of the congealing point thermometer is to transparent
Airshower bottom about 10~15mm.
5. measurement device as described in claim 1, which is characterized in that the transparent airshower is fixed on institute by magnetic sheet
It states on support base.
6. the measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point, comprising:
(1) by sample melting for liquid；
(2) sample is dipped using congealing point thermometer；
(3) the congealing point thermometer with fluid sample is installed on transparent airshower；
(4) the transparent airshower rotated on rotating device is heated, heating intensity is controlled, when thermometer reaches predetermined temperature
Stop heating afterwards, observe the waxy and temperature reading on mercury ball, when the waxy rotation with thermometer mercury ball, reads immediately
Temperature value, the as congealing point of the sample.
7. measuring method as claimed in claim 6, which is characterized in that by sample melting to be sufficiently stirred after liquid.
8. measuring method as claimed in claim 6, which is characterized in that when dipping sample, fluid sample is made to be sticked to thermometer
Mercury bulb.
9. measuring method as claimed in claim 6, which is characterized in that the revolving speed of the rotating device is 2~3s/ circle.
10. measuring method as claimed in claim 6, which is characterized in that same sample carries out replication, takes 2-3 measurement
Congealing point of the average value of value as institute's test specimens.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711470370.1A CN109991261A (en) | 2017-12-29 | 2017-12-29 | The measurement device and measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711470370.1A CN109991261A (en) | 2017-12-29 | 2017-12-29 | The measurement device and measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point |
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|---|---|
| CN109991261A true CN109991261A (en) | 2019-07-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711470370.1A Pending CN109991261A (en) | 2017-12-29 | 2017-12-29 | The measurement device and measuring method of a kind of Fischer-Tropsch wax and pertroleum wax congealing point |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114216927A (en) * | 2021-12-24 | 2022-03-22 | 湖北富邦新材料有限公司 | Method for rapidly detecting melting point of anti-caking agent for chemical fertilizer |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0545312A (en) * | 1991-08-21 | 1993-02-23 | Nippon Shokubai Co Ltd | Automatic freezing-point measuring apparatus |
| CN102445402A (en) * | 2011-10-09 | 2012-05-09 | 唐山德生防水材料有限公司 | Rapid measurement apparatus for total amount of moisture and evaporation loss of petroleum heavy oil components, and method thereof |
| US20170160217A1 (en) * | 2015-12-04 | 2017-06-08 | Exxonmobil Research And Engineering Company | Apparatus for determining the congealing point of a petroleum wax sample and methods therefor |
| CN106814099A (en) * | 2017-01-04 | 2017-06-09 | 中国工程物理研究院化工材料研究所 | Freezing point, fusing point or crystalline temperature automatization test system |
| CN207946381U (en) * | 2017-12-29 | 2018-10-09 | 内蒙古伊泰煤基新材料研究院有限公司 | A kind of measurement device of Fischer-Tropsch wax and pertroleum wax congealing point |
-
2017
- 2017-12-29 CN CN201711470370.1A patent/CN109991261A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0545312A (en) * | 1991-08-21 | 1993-02-23 | Nippon Shokubai Co Ltd | Automatic freezing-point measuring apparatus |
| CN102445402A (en) * | 2011-10-09 | 2012-05-09 | 唐山德生防水材料有限公司 | Rapid measurement apparatus for total amount of moisture and evaporation loss of petroleum heavy oil components, and method thereof |
| US20170160217A1 (en) * | 2015-12-04 | 2017-06-08 | Exxonmobil Research And Engineering Company | Apparatus for determining the congealing point of a petroleum wax sample and methods therefor |
| CN106814099A (en) * | 2017-01-04 | 2017-06-09 | 中国工程物理研究院化工材料研究所 | Freezing point, fusing point or crystalline temperature automatization test system |
| CN207946381U (en) * | 2017-12-29 | 2018-10-09 | 内蒙古伊泰煤基新材料研究院有限公司 | A kind of measurement device of Fischer-Tropsch wax and pertroleum wax congealing point |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114216927A (en) * | 2021-12-24 | 2022-03-22 | 湖北富邦新材料有限公司 | Method for rapidly detecting melting point of anti-caking agent for chemical fertilizer |
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