CN101074910B - Need in-degree device and use in asphalt need in-degree determination - Google Patents

Need in-degree device and use in asphalt need in-degree determination Download PDF

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CN101074910B
CN101074910B CN2006100466331A CN200610046633A CN101074910B CN 101074910 B CN101074910 B CN 101074910B CN 2006100466331 A CN2006100466331 A CN 2006100466331A CN 200610046633 A CN200610046633 A CN 200610046633A CN 101074910 B CN101074910 B CN 101074910B
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pen
ware
temperature
pitch
sample
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CN101074910A (en
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吴佩尊
宁爱民
朱玲
赵丽
马丹
杨梅
景东宇
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China Petroleum and Chemical Corp
Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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Sinopec Fushun Research Institute of Petroleum and Petrochemicals
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Abstract

A penetrator is prepared as forming outline of penetrator by symmetrically cutting off two parts of cylindrical column, setting cut surface to be vertical to top and bottom surfaces of original cylindrical column, setting top and bottom surfaces of cut-off part to be bow form, setting arch height of said bow form to be H and external diameter of cylindrical barrel to be D to make ratio of H to D be 0.05-0.30.

Description

A kind of pen. ware and the application in the pitch penetration test thereof
Technical field
The present invention relates to a kind of pen. ware and the application in the pitch penetration test thereof, is the improvement to the pen. ware of routine, when being used to measure pitch pen., can reach the purpose of fast measuring pitch pen..
Background technology
Petroleum bitumen is a kind of thermoplasticity viscoelastic material, and its rheological property and temperature have substantial connection.Be subjected to stress or during because of temperature change, its state can change.On macroscopic view, during low temperature, not only firmly but also crisp, character and glassy phase were seemingly for pitch; When temperature approached softening point, pitch began to take place viscoelastic deformation, and pitch at this moment is soft, not only flexible but also toughness; Temperature continues to raise, owing to further deformation takes place the trend flow state; When flow deformation was preponderated, pitch began to flow with the liquid of thickness.
In every character index of the quality of standard asphaltic products and usability, the pen. reflection be the sliminess or the soft or hard degree of pitch, be asphaltic products produce and research process in the most basic controlling index.Compare with other index, the rheological property that pen. reflected is more definite, assay method is simpler and more direct, the result is more accurate.Therefore, at present China and many countries in the world remain with penetration number as the graded index of asphaltic products.
As important performance and quality control index, in commercial production and research work, usually need to grasp at any time the penetration number certificate of asphalt sample, so that timely adjusting process condition; When raw material or technology after changing, desire to understand as early as possible and produce or during the situation up to standard of the operation conditions of process of the test and product, convenient relatively and reliable approach also is the penetration number certificate that needs in time to grasp product.
But, at present domestic and international general penetration test method, the time of the process need of determination test is long.Regulation according to GB/T 4509-1998 " pitch penetration test method ", from collect be in the trickling state the heated bitumen sample to determining the pen. result, generally need to wait for 2~2.5 hours, promptly must make the injection test mould---the heated bitumen in the pen. ware, through after the cooling cooling and the temperature conditions processing in two stages of constant temperature of stipulated time, can carry out determination test.If room temperature higher (as in southern summer), or the sliminess of sample is when smaller, and the time of wait is also longer.
For the modernization industry of operation continuously, the time is first preciousness, and what modern industry can not delay most is exactly the time.And waiting for that between the pen. fruiting period, process conditions, the running status of production or test unit all must steadily be kept, and water, electricity, vapour etc. consume as usual, and product again can not be as finished product.Waste is bigger, is that people are undesirable, and this also is the problem that urgency is to be solved that pitch production for a long time and research field are faced.
In order to shorten the time of wait, for these years, people are seeking various approach always, to realize carrying out fast of penetration test.But up to the present, the method for the most general and unique employing is the method for a kind of being referred to as " penetration test fast ".This method is half that artificial cooling cooling and constant temperature time with sample shortens to code requirement, just shorten to 0.5 hour injecting 1~1.5 hour of being stipulated by standard the aerial cooling of heated bitumen cool time in the pen. ware, the constant temperature time in water bath with thermostatic control also shortened to 0.5 hour by 1~1.5 hour.Measure pen. with this fast method, the time of the temperature conditions time ratio code requirement of sample has shortened 1~2 hour, and for the productive capacity that improves commercial plant, the reduction energy and raw-material waste, its original idea is positive, desirable.But the essential defect of this method is exactly the temperature conditions effect problem not in place, incomplete of the sample that causes because the time shortens that fundamentally do not solve, thereby causes the measurement result deviation bigger.Therefore, generally can only be as the reference frame under the case of emergency.In the practical operation, in order to tackle the fast measuring the possibility of result to the misleading of producing or the test technology regulation and control cause, usually to get two parts to testing sample simultaneously, should carry out express method measures, also will carry out standard law measures, and generally be the result that measures with express method with after operator's experience combines, form the preliminary judgement that technological process is regulated and control, treat to be re-used as after standard test method result comes out the final foundation of regulation and control scheme.
The pen. ware that regulation is used in " pitch penetration test method " (GB/T 4509-1998) is cylinder barrel shaped, an end opening, and its xsect is circular (its structural representation is seen Fig. 1).This pen. ware is formed by higher material of heat transfer coefficient such as aluminium, aluminium alloy, copper or stainless steels.
Summary of the invention
The present invention is directed to the deficiency of " penetration test fast " method, proposed a kind of pen. ware and the application in measuring pitch pen. thereof that can fast, accurately measure pitch pen..
Pen. ware of the present invention has following feature:
Face shaping: be equivalent to that the cylinder symmetry is cut two end faces and the bottom surface is arc part, and its tangent plane is perpendicular to the end face and the bottom surface of former cylinder, the remainder of gained is the face shaping of pen. ware of the present invention;
Inner structure: tubular, an end opening;
Dimensional requirement: the arch height that cuts part is h, and the cylinder overall diameter is D, and wherein h and D concern that ratio is greater than 0 and is not more than 0.30, are preferably 0.05~0.30, are preferably 0.18~0.28.
High and overall diameter cylinder of tube of pen. ware of the present invention can adopt those skilled in the art can be used to measure the overall diameter of the high and cylinder of the tube of cylindrical shape pen. ware of pitch pen., usually the high overall diameter with cylinder of the tube of the used cylindrical shape pen. ware of selection standard method.Alleged standard method is a method of measuring pen. by the pen. ware and the condition determination of GB/T 4509-1998 " pitch penetration test method " regulation among the present invention, and the tube of wherein used pen. ware is high to be 35mm, and the cylinder overall diameter is 55mm.
Pin of the present invention is gone into the pen. that ware is used to measure pitch, and its method comprises the pre-service of asphalt sample, the mensuration of pen., and detailed process is as follows:
Phase one: the heated bitumen sample at room temperature leaves standstill and cools 0.5~<1 hour after injecting modified pen. ware, preferred 0.5~0.75 hour, makes the temperature of asphalt sample reduce to room temperature;
Subordinate phase: the pitch of phase one gained and pen. ware are put in the water bath with thermostatic control that is in test temperature constant temperature 0.5~<1 hour, preferred 0.5~0.75 hour, make the temperature of asphalt sample reach test temperature.Wherein the test temperature control accuracy is ± 0.1 ℃, consistent in this precision and the standard method.
The condition determination of pitch pen. can adopt the condition determination of this area routine, condition determination in the common selection standard method, be GB/T 4509-1998 " pitch penetration test method " defined terms: with standard pin in a constant load, temperature, vertically penetrate the depth representing of pitch sample in the time, unit is 1/10mm.Modified pen. ware of the present invention can be applied to the mensuration of road asphalt pen., and wherein the general assembly (TW) of standard pin, pin connecting rod and additional weights is (100 ± 0.05) g, and test temperature is 5 ℃~35 ℃, and the time is 5 seconds.Generally used test temperature is one or more in 5 ℃, 10 ℃, 15 ℃, 25 ℃, 30 ℃, 35 ℃.
Modified pen. ware of the present invention, also can be applied to other specific penetration test condition that the test of buildings waterproof pitch and various special asphalt is adopted, test condition is with GB/T 4509-1998 standard test method, as the specified temp of regulations such as buildings waterproof pitch or various special asphalts among the GB/T 4509-1998 and the penetration test under the specific load.
Phase one heated bitumen sample is meant the asphalt sample to be measured of picking up from different production or technological process, being in the trickling state.
The used pen. ware of the present invention is to have made improvement on the basis of cylindrical shape pen. ware used in conventional method, is about to cylinder barrel shaped and has made into to be equivalent to the cylinder barrel shaped symmetry has been cut the shape that two end faces and bottom surface are gained after the arc part.After the improvement, as a whole, though the key dimension of pen. ware---diameter and high not change, but because its alteration of form, specific surface area has increased relatively, and the heat transfer area that the unit mass sample is had has also increased relatively, thereby rate of heat transfer has improved.Again from the inner structure of pen. ware and since symmetry cut a part outside the efficiency test zone, thereby make the heat-transfer path of different parts sample that in various degree shortening all be arranged, and more near the centre, distance shortens manyly more.Theoretically, being positioned at the rate of heat transfer of pen. ware centre sample, is the key of influence and the total rate of heat transfer of constraint sample.Have only the rate of heat transfer that improves the centre sample, and make it to reach as early as possible requirement, then the bulk temperature conditioning process of sample could be accelerated, and the problem that shortens the time could solve.This shows, the present invention adopts modified pen. ware, not only the heat-transfer path at each position is more reasonable, and the corresponding increase of heat transfer area that has of unit mass sample, thereby shortened the temperature conditions time greatly, can reach half of used time of standard method, increase substantially work efficiency thus.
The manufacturing materials of the modified pen. ware that the present invention is used is used identical with conventional method, can use the higher materials of coefficient of heat conductivity such as aluminum or aluminum alloy, copper, stainless steel, also can use materials such as glass, the most handy aluminum or aluminum alloy.
The inventive method is by conventional " pitch penetration test method " employed pen. ware is improved, satisfying under the prerequisite of testing requirements, by increasing the specific surface that conducts heat, reduce sampling amount, shorten heat-transfer path, improved the heat transfer efficiency of sample, fundamentally solved the matter of time that shortens the sample temperature conditioning, shortened the penetration test time, the simultaneously measured pen. and the pen. of standard method gained are basic identical.Require from the degree of accuracy of test findings, the penetration number maximum deviation of the penetration number of the inventive method gained and standard method gained is 2 units, in the error range of GB/T 4509-1998 standard-required.
Modified pen. ware of the present invention, the quality testing station (center) that can be used for asphaltic products manufacturing enterprise, the laboratory of pitch technological development and research, the laboratory of highway and municipal sector, and quick penetration test is carried out to asphalt sample in the laboratory of working-yard such as pave the way.
Description of drawings
Fig. 1 is the structural representation of standard pin in-degree ware used in the GB/T 4509-1998 standard; Fig. 2 is the structural representation of pen. ware of the present invention.Fig. 3 is the bottom surface (or end face) of the improved pen. ware of the present invention, and Fig. 4 is the size synoptic diagram of pen. ware of the present invention bottom surface, and wherein D is a diameter, and h is the bow height that symmetria bilateralis is clipped the part bottom surface.
Embodiment
The inventive method adopts modified pen. ware, remove the temperature conditions time of sample, the heated bitumen that promptly injects the pen. ware at room temperature the cooling cooling and outside the constant temperature time in water bath with thermostatic control all shortens, all the other steps are all undertaken by GB/T 4509-1998 standard.
Embodiment one
25 ℃ of pen. almost is that each asphalt sample must be surveyed as the graded index of most asphaltic productses.The key dimension of the modified pen. ware that present embodiment uses is: cylinder overall diameter D=55mm, the high 35mm of tube bends high h: diameter D=0.18.
Present embodiment chosen the different process preparation the different soft and hard degree straight asphalt, SBS modified bitumen and added the modified bitumen sample that various chemical modifiers are made, be experiment mould with standard ware and improvement ware respectively, measure their 25 ℃ of pen.s.Wherein, the mensuration process of standard ware is carried out according to method for normalizing GB/T4509-1998, and be 1 hour the cool time of wherein lowering the temperature, and constant temperature time is 1 hour; Adopt improvement ware of the present invention, except that lower the temperature cool time and constant temperature time have shortened 0.5 hour than the employing standard used time of ware respectively, all the other processes are also carried out according to method for normalizing GB/T 4509-1998, the results are shown in table 1.
The measurement result of table 1 embodiment 1
By table 1 as seen: the measured value that improves ware and standard ware mostly differs 1~2 unit, and in normal error at measurment scope, its mean value differs 1 unit at most, and relative deviation is all less than 1%.Therefore, the inventive method adopts improved pen. ware, and measured penetration number is consistent with improving preceding measured value substantially.
Embodiment two
Measure the penetration number of same sample under a plurality of different temperatures, and the coefficient R by linear regression Calculation pen. result, and weigh penetration test result's order of accuarcy with the degree that R satisfies the respective specified value, be to introduce mathematical statistics method checking penetration test a kind of approach of accuracy as a result in recent years.In the present embodiment, when adopting the standard ware, its mensuration process is carried out according to method for normalizing GB/T 4509-1998, and be 1 hour the cool time of wherein lowering the temperature, and constant temperature time is 1 hour; The key dimension of the modified pen. ware that present embodiment uses is: cylinder overall diameter 55mm, the high 35mm of tube, bend high h: diameter D=0.28, except that lower the temperature cool time and constant temperature time have shortened 0.5 hour than the employing standard used time of ware respectively, all the other processes are also carried out according to method for normalizing GB/T 4509-1998.Table 2 has been listed 3 the penetration test results and the linear regression Calculation result of same sample.From the result that two kinds of pen. wares record, the measured value under the relevant temperature, the equal basically identical of mean value, coefficient R is very approaching, and far above 0.997 regression Calculation required value.As seen, modified pen. ware has shortened in the time under the situation of half, is identical to the effect of the temperature conditions processing of sample with the standard ware.
Pen. result's contrast under the same sample multi-point temp of table 2
Embodiment three
The key dimension of the modified pen. ware that present embodiment uses is: cylinder overall diameter D=55mm, the high 35mm of tube bends high h: diameter D=0.05.Adopt standard ware and improvement ware that asphalt sample is carried out penetration test respectively, except following condition, other operating conditions is all identical with standard method with step.When wherein adopting the standard ware, at room temperature cooling cool time and the constant temperature time in water bath with thermostatic control are 1.0 hours; , adopting when improving ware, at room temperature cooling cool time and the constant temperature time in water bath with thermostatic control are 0.75 hour, and measurement result sees Table 3.
The measurement result of table 3 embodiment three
Figure G06146633120060608D000091
Embodiment four
Compare with " pitch penetration test method " (GB/T 4509-1998), " fast penetration test " main deficiency of method is the temperature conditions treatment effect of sample is failed to reach the requirement of standard.The inventor finds in practice, by temperature conditions time of GB/T 4509-1998 regulation sample is lowered the temperature after cooling, constant temperature handle, penetration test result's maximum deviation, repeatability, repeatability all in the energy compliant to the requirement of precision.And temperature conditions processing time during less than setting, measurement result mostly can not meet the requirement of precision.The temperature conditions time of stipulating in the description standard method is to satisfy the most basic time of test findings accuracy.When using standard pin in-degree ware to carry out penetration test, the temperature conditions time can not be shortened arbitrarily.
In the present embodiment, standard ware and improvement ware and sample cooling cool time and the constant temperature time in water bath with thermostatic control at room temperature thereof are all shortened to 0.5 hour, and with the standard ware by the standard test method, promptly sample cooling cool time and the constant temperature time in water bath with thermostatic control at room temperature is the pen. result who measured in 1 hour and compares.The result shows: the equal overgauge value of result that the standard ware is measured, and the measurement result of improvement ware, and then with the standard value basically identical.This just further proves from another point of view: modified pen. ware is reliable to the temperature conditions treatment effect of testing sample, when needing in the practical application, can replace the standard ware that asphalt sample is carried out quick penetration test, thereby realize pen. fast measuring truly.
The key dimension of the modified pen. ware that uses in the present embodiment is: cylinder overall diameter D 55mm, the high 35mm of tube bends high h: diameter D=0.23.Comparative test result is listed in table 4.
The comparative test result of table 4 embodiment four
Figure G06146633120060608D000101

Claims (12)

1. pen. ware is characterized in that this pen. ware has following characteristics:
(1) face shaping: the cylinder symmetry is cut two parts, and its tangent plane is perpendicular to the end face and the bottom surface of former cylinder, and the end face and the bottom surface that cut part are arc, and the remainder of gained is the face shaping of this pen. ware;
(2) inner structure: tubular, an end opening;
(3) dimensional requirement: the arc pitch of arch that cuts part is h, and the cylinder overall diameter is D, and wherein h and D ratio are greater than 0 and are not more than 0.30.
2. according to the described pen. ware of claim 1, it is characterized in that the h of described pen. ware and D ratio are 0.05~0.30.
3. according to the described pen. ware of claim 1, it is characterized in that the h of described pen. ware and D ratio are 0.18~0.28.
4. according to the described pen. ware of claim 1, it is characterized in that the high and cylinder overall diameter D of the tube of described pen. ware is the setting that adopts among State Standard of the People's Republic of China's " GB/T4509-1998 pitch penetration test method ".
5. according to the described pen. ware of claim 1, it is characterized in that the high 35mm of being of tube of described pen. ware, cylinder overall diameter D is 55mm.
6. a method of measuring pitch pen. comprises the pre-service of asphalt sample, the mensuration of pen., it is characterized in that the preprocessing process of asphalt sample is as follows:
Phase one: the heated bitumen sample at room temperature leaves standstill and cools 0.5~<1 hour after injecting the arbitrary described pen. ware of claim 1~5, makes the temperature of asphalt sample reduce to room temperature;
Subordinate phase: the pitch of phase one gained and pen. ware are put in the water bath with thermostatic control that is in test temperature constant temperature 0.5~<1 hour, make the temperature of asphalt sample reach test temperature.
7. method according to claim 6, the time of cooling that it is characterized in that the described phase one is 0.5~0.75 hour, the used constant temperature time of subordinate phase is 0.5~0.75 hour.
8. method according to claim 6 is characterized in that the temperature control precision of the water bath with thermostatic control of described subordinate phase is ± 0.1 ℃.
9. method according to claim 6 is characterized in that described pen. is to adopt the condition determination among State Standard of the People's Republic of China's " GB/T4509-1998 pitch penetration test method " to measure.
10. method according to claim 6, it is characterized in that described modified pen. ware is applied to the mensuration of road asphalt pen., wherein the general assembly (TW) of standard pin, pin connecting rod and additional weights is (100 ± 0.05) g, and test temperature is 5 ℃~35 ℃, and the time is 5 seconds.
11. method according to claim 10 is characterized in that described test temperature is one or more in 5 ℃, 10 ℃, 15 ℃, 25 ℃, 30 ℃, 35 ℃.
12. method according to claim 6 is characterized in that described modified pen. ware is applied to the mensuration of the specific pen. that buildings waterproof pitch and various special asphalt adopted.
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CN102768170A (en) * 2012-07-24 2012-11-07 沈阳新一代信息技术有限公司 Monitoring device for asphalt penetration test and method for detecting asphalt label
CN108169073A (en) * 2017-10-30 2018-06-15 甘肃达利食品有限公司 A kind of detection method of potato full-powder stability
CN108225893A (en) * 2017-12-29 2018-06-29 广州市德隆化工贸易有限公司 A kind of penetration test former of wax material and the needle penetration highly effective testing method based on it

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Publication number Priority date Publication date Assignee Title
CN87208346U (en) * 1987-05-21 1987-12-31 广东省交通科学研究所 Optoelectronic pitch penetrometer for asphalt

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN87208346U (en) * 1987-05-21 1987-12-31 广东省交通科学研究所 Optoelectronic pitch penetrometer for asphalt

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JP特开2001-141630A 2001.05.25
石油大学(华东)重质油研究所.GB/T4509-1998沥青针入度测定法.中华人民共和国国家标准.1998,1-3. *

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