CN1037548C - 对沥青中添加剂进行标记和鉴定 - Google Patents
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Abstract
将标记物质加入沥青所用的添加剂中,这些添加剂典型地是一种抗剥离剂。将标记的添加剂与沥青组合物的其它组分混合,然后在300F(149℃)或更高的温度进行熔融处理,获得沥青组合物。通过将组合物的沥青部分溶于与水不混溶的溶剂中,然后用酸性水溶液萃取出标记物质,并用重氮基化合物显示颜色来鉴定标记物质的存在,因而添加剂的存在。
Description
本发明涉及标记沥青中的添加剂(以下简称沥青添加剂,特别的如抗剥离剂)以及石灰和填料进行标记的方法。
沥青组合物,例如用于铺路的沥青混凝土或铺顶的沥青组合物包含沥青水泥和集料。典型的集料为天然或合成的含各种筛目尺寸或特定筛目尺寸的砂和砾石。沥青可以有各种级别,例如,硬级别沥青用于在较暖和气候下铺路,而软级别沥青用于在较冷气候下铺路。沥青中可以加入聚合物材料例如橡胶或胶乳来进行改性。同样地,集料的粒度分布和种类可以有很大的差别,视用途而异。在用于铺路的沥青混凝土中,集料占绝大部分,其典型含量约为95%(重量),而沥青部分占剩余的5%(重量)。
如在U.S.Pat.Nos.4,775,419,4,430,127,4,639,273,4,743,304和5,037,474中所述(已参考引用结合入本文中),大部分对沥青组合物耐久性主要起限制作用的因素是沥青部分和集料之间的粘合强度,此粘合强度可因水(最初存在于集料中的水或沥青组合物随后所接触的水)而减弱。因此,如上述引用的专利所述,可将抗剥离剂加入沥青部分中。典型的抗剥离剂是一种有机聚胺(例如用于U.S.Pat.No.4,430,127),但可以是许多种其它化合物或一些化合物的混合物。U.S.Pat.No.4,775,419揭示了使用金属胺配合物。U.S.Pat.No.4,430,127揭示了使用环氧化聚胺。U.S.Pat.No.4,639,273揭示了使用胺、聚胺和酰胺的甲醛加成物。U.S.Pat.No.4,743,304揭示了使用咪唑啉、聚胺、烷氧基化聚胺、氨基羧酸酯、酰胺-胺以及它们的混合物。U.S.Pat.No.5,037,4747则揭示了使用一种环氧化合物与磷酸或磷酸偏酯的反应产物。其它材料,例如加入集料中的石灰、或填料如纤维素或波特兰水泥,也可加入以提高沥青组合物的强度和耐久性。
沥青组合物的使用寿命在很大程度上依赖于加入的添加剂,特别是抗剥离剂,还有石灰和填料。因此,合同(例如州政府铺路合同),一般会规定所用添加剂的种类和用量。不幸的是,一旦沥青组合物的各组分相互混合后,没有特别好的方法来确定抗剥离剂和其它添加剂的含量。添加剂如抗剥离剂在沥青混凝土中只占很少的比例。抗剥离剂的典型含量约为沥青部分的0.2-5.0%(重量),而沥青部分又只占沥青混凝土的5%(重量)。尽管添加剂是含量少的组分,基于每磅的费用,它们通常比集料或沥青本身贵得多。诚然,在混合沥青组合物的组分时会发生无意的差错。但不幸的是,可能不诚实的承包方会出于经济上的刺激而在沥青组合物中减少或不用抗剥离剂或其它添加剂,或使用比合同规定的更便宜级别的抗剥离剂。由于尚无测定添加剂量的有效实验方法,就增加了在这方面弄虚作假的趋势。人们知道还有这种情况:承包方即使事先并无欺骗的意图,但在用完了添加剂后,仍继续进行铺路施工。
对铺路沥青提出要求的承包方(例如州政府或国家的部)希望的是有一种监测添加剂含量的方法,实际上用来确保其与合用规定的条款相符。这种监测可以趁沥青部分仍是热的时候进行取样,或者对已硬化的沥青混凝土(热混合沥青)进行取样,其时机或者是铺路之时,或者在以后的某个时候(如果检测方法必须如此的话)。
在研究测量抗剥离剂的方法方面,努力大多集中于化学分析。这些努力迄今获得的一些实验方法都是实施起来比较麻烦的,很难定量,而且通常不能辨别各种品种的抗剥离剂,本发明则涉及对沥青添加剂进行标记并鉴定已标记添加剂的方法。
按本发明,将特定结构式的标记物质加入沥青添加剂中,用于形成沥青组合物的原料的混合物在通常条件下进行处理,例如在约300°F(149℃)和更高的温度下处理,随后冷却形成硬化沥青组合物。从热的混合物或硬化沥青组合物取样,然后将沥青部分溶于一种合适的溶剂。再将标记物质以酸性水溶液的形式萃取出来,使其与重氮其化合物反应产生很强的颜色。
在本专利申请中,对下述术语作如下定义:
“沥青”应广义地指不仅包括真沥青,而且还包括其它有关的沥青材料,如用于铺路、屋顶等的煤焦油。
“沥青组合物”应指任何含沥青的组合物,包括指含集料或其它不溶物的组合物,或指不含集料或其它不溶物的组合物。
“沥青混凝土”应指任何含集料或其它不溶物的沥青组合物。
“沥青部分”应指沥青组合物中,含有沥青和任何与沥青可混溶的物质(包括抗剥离剂和标记物质)的那一部分。
用于本发明过程的标记物质乃是在授予RiChard Orelup的U.S.Pat No.4,209,302中所述的化合物,在此参考引用加以说明,具体地说,该类标记物质是下述结构式的化合物: 和
其中R1和R2为氢或含1至20个碳原子的烷基,R3为含1至8个碳原子的烷基。如U.S.Pat.No.4,209,302所述,这些化合物先前已开始用作石油的标记物质。用于标记石油的物质几乎总是加入通常从不显著高于室温的精炼石油的。而任何用于沥青添加剂的标记物质则必须受到沥青组合物进行热加工处理的高温。由于绝大多数石油标记物质在沥青处理的温度即高于约300°F(149℃)和更高并且通常约350°F(177℃)和更高的温度下是不稳定的,因此它们不宜作标记沥青之用。绝大多数石油标记物质在沥青组合物处理过程中,其全部或大部将被破坏。然而,已经发现用于本发明的化合物在沥青处理的温度下是稳定的,而且在现场长时间过程(此时沥青发生着氧化)中,这种化合物在沥青组合物中都是可以检测出来的。
还令人惊奇的是含有本发明标记物质和一种聚 胺抗剥离剂的沥青组合物可以与不含此标记物质的该组合物区别出来。本发明标记物质在化学上类似于聚胺抗剥离剂,因为该标记物质含有两个胺基。然而,未作标记的沥青组合物在作鉴定试验时不产生颜色,而作了标记的组合物在试验时产生很强的颜色。此试验通常是定量的,因为多次试验已显示出可检测的加入沥青中的标记物质的量在10%范围之内。这个相对定量的试验不仅可用来确定加入的添加剂是否正确,而且能确定所加入添加剂的量是否正确。
通常大多数要作标记的添加剂是有机抗剥离剂。然而,对任何添加剂,例如石灰或填料例如波特兰水泥或纤维素也可进行标记。以集料重量为基准,石灰的典型用量为1-2%,波特兰水泥为0.5-3%,纤维素则达10%。例如,委托铺路工程的某一州的当局会周期性地改变要被标记的添加剂以逐个检查承包方是否采用了规定量的各组份。因为上述结构式的标记物质是以类似方式萃取和显色的,通常只有一种添加剂能作标记并检测出来。然而,有可能采用上述通式的两种标记物质用来标记两种不同的添加剂,只要这两种标记物质能产生可用分光光度测定区别的不同吸收峰的两种颜色。
可以从中萃取并显色的上述结构式的标记物质的溶液,其标记物质的含量可低至0.5ppm(重量/体积)。在本发明的方法中,可以从中萃取标记物质并显色的溶液为沥青部分溶于溶剂的溶液。因此,加入添加剂中标记物质的量应予计算,使得沥青部分溶于溶剂的溶液中标记物质达到所需的浓度。尽管可检测出的标记物质的浓度是0.5ppm(重量/体积),但较好地是采用足够多的标记物质,使沥青部分在溶剂中的溶液含有至少约10ppm的标记物质。这就使得试验能更定量一些并可以使检测和鉴定见效,如果虽然使用了所需的添加剂但其用量低于规定的话。在抗剥离剂中,标记物质的典型用量约为0.5-5%(重量),1-2%(重量)则更好。抗剥离剂的典型用量约为沥青部分的0.2-5%(重量)。在试验时,所用溶剂的体积至少约为沥青部分体积的3倍,以充分溶解沥青部分。为了有效更好地显色,溶剂的体积很少大于沥青部分体积的10倍左右。若将标记物质加入石灰或填料中,可相对于添加剂的使用量和沥青部分在溶剂的溶液中所希望标记物质的量来计算标记物质的用量。
本发明的标记物质不能直接从沥青部分中萃取出来,这样就需要减少溶剂中的沥青部分。适用的溶剂是那些容易溶解沥青部分,而且还是与水不混溶的溶剂。这些合适的溶剂包括甲苯、柑桔溶剂、二甲苯、煤油、1,1,1-三氯乙烷、三氯乙烯以及它们的混合物。
可在新混合的沥青组合物样品或冷却固化组合物的样品中测知标记的存在。若需要试验热混合物,可由其取样出一定体积的组合物,然后通常令其冷却,至少冷至低于对该样品进行溶解处理的溶剂的沸点,所试验的沥青组合物的体积应考虑到沥青组合物中的绝大部分是集料,而只有沥青部分才能溶于溶剂中。然后根据算出的在沥青组合物中沥青部分的量计算加入的溶剂量,对于添加剂含量的最精确则量,在沥青部分溶解于溶剂后所剩余的集料和其它不溶物的体积应随后测定之。
然后用酸性水溶液萃取出标记物质,再用一种重氮基化合物显色。萃取溶液的pH值最好约为4或较低些。所用酸性水溶液的体积应足以基本上萃取出所有的标记物质,但宜在需要的范围内尽量小,使得标记物质的浓度较大,以显示最强的颜色。萃取剂溶液的体积与沥青部分溶于溶剂的溶液的体积之典型比例约为1∶10至1∶1,虽然可采取任何比例,只要显出的颜色足以检测出来。萃取本发明方法的标记物质可用乙酸/水溶液,或其它酸如丙酸、HCl或甲磺酸的溶液。为了更好地从溶剂相中分离出水相,可加入少量的抗乳化剂。
酸性的水萃取剂可以含有显色必需的重氮基化合物,或者重氮基化合物可在分开的显色步骤中加入。该重氮基化合物可以是能使标记物质的萘环重氮化的任何化合物。重氮基化合物的用量对于存在于沥青组合物中标记物质的量在化学计量上是过量的。为了便于使试验物质在此鉴定用途上产生可预见的结果最好使用一种稳定化的重氮基化合物,其例子包括2一氯-4-硝基苯胺、2-氯-苯胺、4-氯-苯胺、2-硝基苯胺,但并不限于这些化合物。
在加入重氮基化合物情况下显示颜色,这个事实本身是对存在标记物质的一个定性检验,因此也就是所规定添加剂的定性检验。对于定量测定,需要对显出的颜色进行分光光度测量。规定添加剂的量则可由添加剂中标记物质的浓度、沥青组合物中沥青部分的体积、用于溶解沥青部分的溶剂的体积以及萃取液/显色剂溶液的体积容易地计算出来。
下面,将用一些特定的实施例对本发明作更详细的描述。
实施例1
为了显示对沥青添加剂进行标记,然后对沥青组合物中的标记物质进行检测的可行性,进行了下述实验。将3.3%(重量)的本发明一种标记物质即1-(4-吗啉代)-3-(α萘氨基)-丙烷加入96.7%的抗剥离剂中,该抗剥离剂为聚胺的混合物,其商品名为Pave Bond Lite。将99份AC-20沥青加热至300°F(149℃),然后加入1份已标记的抗剥离剂并混合之。将此沥青组合物冷却至室温。将5体积份沥青组合物用95体积份二甲苯进行溶解处理。将20cc沥青在二甲苯中的溶液倒入-125ml分液漏斗中。然后,加入10cc含20份氯化铵和20份丙酸的水溶液,并混合2分钟。加入0.1ml抗乳化剂(PetrotecR 7400)。混合物静置5分钟后,将底层水相放入50ml量筒。在水相中加入0.1ml α-氯-苯胺,轻微摇动所得溶液。明亮的蓝红色显示了有标记物质存在。
实施例2
制备了一种压实的沥青混凝土,它包含:
94.1%集料
5.8705%沥青水泥
0.0292%PAVA BOND LITE*
0.0002%实施例1的标记物质
在175°F(80℃)下将此压实沥青混凝土加热直至软化。将100g此软化的沥青混凝土置于容量为1升的烧杯中,加入45ml BiogenicElectrosafe**,边搅拌边加热,直至沥青混凝土溶解(约30分钟)。将溶液在一重力过滤器上进行倾析,然后将溶解后剩下的集料在过滤器上面用65ml Biogenic Electrosafe洗涤之。将滤液转移至100ml分液漏斗中。再加入45ml Extractant A 20***,轻微调拌使之分层,放掉清澈的底层水相,硝基-氯-苯胺在乙酸和硫酸中的溶液,就显示了淡粉红色。
*Morton International,lnc所售的聚胺抗剥离剂
**含d-柠檬油精来自Rochester Midland的石油馏出物的未氯化溶剂
***50g氯化铵,50g乙酸,100ml水
虽然本发明已用上述的一些较佳实施例进行了描述,但在不偏离本发明范围的情况下,可以进行对于本技术的熟练人员来说显而易见的各种改进。
本发明的各种特征在下述权利要求书中予以阐明。
Claims (7)
2.如权利要求1所述的方法,其特征在于,所述添加剂为抗剥离剂。
3.如权利要求2所述的方法,其特征在于,所述抗剥离剂是聚胺。
4.如权利要求1所述的方法,其特征在于,所述添加剂为石灰。
5.如权利要求1所述的方法,其特征在于,所述添加剂为填料。
6.如权利要求5所述的方法,其特征在于,所述填料为波特兰水泥。
7.如权利要求5所述的方法,其特征在于,所述添加剂为纤维素
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US08/053,256 | 1993-04-26 | ||
US08/053,256 US5306343A (en) | 1993-04-26 | 1993-04-26 | Tagging and identifying asphalt additives |
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CN1094735A CN1094735A (zh) | 1994-11-09 |
CN1037548C true CN1037548C (zh) | 1998-02-25 |
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EP (1) | EP0622631B1 (zh) |
JP (1) | JP2558067B2 (zh) |
CN (1) | CN1037548C (zh) |
AU (1) | AU653903B1 (zh) |
CA (1) | CA2114896C (zh) |
DE (1) | DE69422332T2 (zh) |
NO (1) | NO302707B1 (zh) |
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US5519073A (en) * | 1995-06-21 | 1996-05-21 | Shell Oil Company | Process for the preparation of a phosphoric-acid-containing asphalt/polymer mixture and resulting asphalt composition thereof |
US5759857A (en) * | 1996-09-26 | 1998-06-02 | Amoco Corporation | Leak detection using chemical markers |
US5902750A (en) * | 1997-08-07 | 1999-05-11 | Morton International, Inc. | Tagging of waterborne compositions with oil-soluble markers |
US6080213A (en) * | 1998-03-18 | 2000-06-27 | Morton International, Inc. | Stabilized aqueous diazo solutions |
AU707140B1 (en) * | 1998-03-18 | 1999-07-01 | Morton International, Inc. | Stabilized aqueous diazo solutions |
US6414056B1 (en) | 1998-05-08 | 2002-07-02 | Exxonmobil Research And Engineering Company | Asphalt compositions and method for making (LAW617) |
FR2781884B1 (fr) * | 1998-07-29 | 2001-03-30 | Colas Sa | Procede et produit pour marquage de composition de revetement routier et composition correspondante |
DE19845474C2 (de) * | 1998-10-02 | 2002-02-07 | Carl Ungewitter Trinidad Lake | Verfahren zum Nachweisen oder quantitativen Bestimmen von Zusatzstoffen zu Asphalt |
DE10004402C2 (de) * | 1998-10-02 | 2002-03-07 | Carl Ungewitter Trinidad Lake | Verfahren zum Nachweisen oder quantitativen Bestimmen von Zusatzstoffen zu Asphalt |
DE19917002A1 (de) * | 1999-04-15 | 2000-10-26 | Martin Lohe | Verfahren zur Identifizierung eines Produktes |
WO2001057517A2 (de) * | 2000-02-02 | 2001-08-09 | Carl Ungewitter Trinidad Lake Asphalt Gmbh & Co. Kg | Verfahren zum nachweisen oder quantitativen bestimmen von zusatzstoffen zu asphalt |
US7098034B2 (en) * | 2002-12-23 | 2006-08-29 | Instrotek, Inc. | Systems and methods for assessing the presence of and/or the level of anti-stripping constituents in asphalt binders or asphalt mixtures |
US9751812B2 (en) * | 2014-05-30 | 2017-09-05 | Elwha Llc | Taggant for cement authentication |
CN114479488A (zh) * | 2020-10-27 | 2022-05-13 | 中国石油化工股份有限公司 | 一种抗剥落剂及其制备方法和应用 |
WO2024073457A1 (en) | 2022-09-28 | 2024-04-04 | Dow Global Technologies Llc | Water miscible fluorescent monomer as marking in a waterborne coating |
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DE2627078A1 (de) * | 1976-06-16 | 1977-12-22 | Licencia Talalmanyokat | Verfahren und einrichtung zur bitumenextraktion |
US4209302A (en) * | 1979-05-10 | 1980-06-24 | Morton-Norwich Products, Inc. | Marker for petroleum fuels |
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US2386867A (en) * | 1942-12-08 | 1945-10-16 | Nostrip Inc | Bitumen treating agent |
US4430127A (en) * | 1981-10-21 | 1984-02-07 | Carstab Corporation | Epoxylated amine asphalt anti-stripping agent |
US4775419A (en) * | 1983-08-12 | 1988-10-04 | Morton Thiokol, Inc. | Metal amine complexes for improving the bond strength properties of asphalt |
US4639273A (en) * | 1983-05-06 | 1987-01-27 | Morton Thiokol, Inc. | Asphalt-adhesion improving additives prepared by formaldehyde condensation with polyamines |
US4743304A (en) * | 1983-12-14 | 1988-05-10 | Morton Thiokol, Inc. | Asphalt antistripping agents containing organic amines and Portland cement |
US5037474A (en) * | 1989-11-27 | 1991-08-06 | Morton International, Inc. | Bitumen antistripping agent |
-
1993
- 1993-04-26 US US08/053,256 patent/US5306343A/en not_active Expired - Fee Related
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1994
- 1994-02-03 CA CA002114896A patent/CA2114896C/en not_active Expired - Fee Related
- 1994-02-08 AU AU54939/94A patent/AU653903B1/en not_active Ceased
- 1994-02-09 EP EP94300951A patent/EP0622631B1/en not_active Expired - Lifetime
- 1994-02-09 DE DE69422332T patent/DE69422332T2/de not_active Expired - Fee Related
- 1994-02-28 NO NO940688A patent/NO302707B1/no not_active IP Right Cessation
- 1994-03-22 CN CN94103223A patent/CN1037548C/zh not_active Expired - Fee Related
- 1994-04-14 JP JP6075739A patent/JP2558067B2/ja not_active Expired - Lifetime
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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DE2627078A1 (de) * | 1976-06-16 | 1977-12-22 | Licencia Talalmanyokat | Verfahren und einrichtung zur bitumenextraktion |
US4209302A (en) * | 1979-05-10 | 1980-06-24 | Morton-Norwich Products, Inc. | Marker for petroleum fuels |
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Publication number | Publication date |
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NO940688D0 (no) | 1994-02-28 |
CN1094735A (zh) | 1994-11-09 |
NO302707B1 (no) | 1998-04-14 |
EP0622631A3 (en) | 1996-05-08 |
AU653903B1 (en) | 1994-10-13 |
JP2558067B2 (ja) | 1996-11-27 |
NO940688L (no) | 1994-10-27 |
US5306343A (en) | 1994-04-26 |
EP0622631B1 (en) | 1999-12-29 |
DE69422332D1 (de) | 2000-02-03 |
CA2114896A1 (en) | 1994-10-27 |
CA2114896C (en) | 1998-08-25 |
DE69422332T2 (de) | 2000-05-25 |
JPH06324030A (ja) | 1994-11-25 |
EP0622631A2 (en) | 1994-11-02 |
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