WO2016161763A1 - 一种用于沥青路面的温敏型抗冻材料及其制备方法 - Google Patents

一种用于沥青路面的温敏型抗冻材料及其制备方法 Download PDF

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WO2016161763A1
WO2016161763A1 PCT/CN2015/089609 CN2015089609W WO2016161763A1 WO 2016161763 A1 WO2016161763 A1 WO 2016161763A1 CN 2015089609 W CN2015089609 W CN 2015089609W WO 2016161763 A1 WO2016161763 A1 WO 2016161763A1
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temperature
chloride
asphalt pavement
temperature sensitive
sensitive
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PCT/CN2015/089609
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English (en)
French (fr)
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王昆
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常州履信新材料科技有限公司
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Priority to US15/317,124 priority Critical patent/US9682889B2/en
Publication of WO2016161763A1 publication Critical patent/WO2016161763A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C04B22/12—Acids or salts thereof containing halogen in the anion
    • C04B22/124—Chlorides of ammonium or of the alkali or alkaline earth metals, e.g. calcium chloride
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/10—Coating or impregnating
    • C04B20/1018—Coating or impregnating with organic materials
    • C04B20/1029—Macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C04B22/16—Acids or salts thereof containing phosphorus in the anion, e.g. phosphates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/10—Carbohydrates or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • C04B24/126—Urea
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
    • C04B26/02—Macromolecular compounds
    • C04B26/26—Bituminous materials, e.g. tar, pitch
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
    • E—FIXED CONSTRUCTIONS
    • E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
    • E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
    • E01C11/00—Details of pavings
    • E01C11/24—Methods or arrangements for preventing slipperiness or protecting against influences of the weather
    • E01C11/245—Methods or arrangements for preventing slipperiness or protecting against influences of the weather for preventing ice formation or for loosening ice, e.g. special additives to the paving material, resilient coatings
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/0075—Uses not provided for elsewhere in C04B2111/00 for road construction
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/76—Use at unusual temperatures, e.g. sub-zero
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch

Definitions

  • the invention belongs to the technical field of road pavement anti-freezing and deicing, in particular to a temperature-sensitive anti-freezing material for asphalt pavement and a preparation method thereof.
  • the traditional method of removing snow and ice is mainly to spread the snow melting agent, or to use the mechanical-based and artificial-assisted operation methods to remove the snow from the surface of the road and achieve the purpose of melting snow and suppressing ice.
  • these measures have great limitations in terms of environmental protection, mobility, and cost.
  • the active deicing technology is to add antifreeze and deicing materials to the asphalt mixture. This technology plays a role in reducing the freezing point of the pavement through the chloride in the asphalt pavement.
  • the low maintenance cost has been widely promoted in developed regions such as Europe and Japan.
  • the technical problem to be solved by the present invention is that in the prior art, the chloride in the pavement asphalt material is subjected to wind and rain for a long time, especially in the high temperature season, the chloride is easily released from the road surface quickly, resulting in chloride on the road.
  • the utilization rate of antifreeze and deicing is not high.
  • the technical solution adopted by the present invention is:
  • a temperature-sensitive anti-freezing material for asphalt pavement that is, a granular double-layer composite material formed by coating a core material chloride with a chloride as a core material and a temperature sensitive agent as a coating film,
  • the components of the composite material are calculated in parts by weight, 75-95 parts of chloride, 5-20 parts of temperature sensitive agent,
  • the chloride is one or a mixture of two or more of sodium chloride, calcium chloride, and magnesium chloride.
  • composition of the temperature sensitive agent is calculated as a percentage by weight, 6-10% of a polyphenylene ether having a molecular weight of 2000, 40-55% of a polypropylene oxide having a molecular weight of 2000-6000, and the balance being glycerol trilaurate.
  • the temperature-sensitive slow release type antifreeze and deicing composite material for the asphalt pavement further comprises a corrosion inhibitor, that is, a rust inhibitor, and the composite material is a mixture of a chloride and a rust inhibitor as a core material, and is heated.
  • a corrosion inhibitor that is, a rust inhibitor
  • the composite material is a mixture of a chloride and a rust inhibitor as a core material, and is heated.
  • the components of the composite material are calculated in parts by weight,
  • the chloride is one or a mixture of two or more of sodium chloride, calcium chloride, and magnesium chloride.
  • composition of the temperature sensitive agent is calculated as a percentage by weight, 6-10% of a polyphenylene ether having a molecular weight of 2000, 40-55% of a polypropylene oxide having a molecular weight of 2000-6000, and the balance being glycerol three laurel Acid ester.
  • the sodium hexametaphosphate used is a white powder, and the pass rate of the 0.1 mm square sieve is more than 85%.
  • the sodium gluconate selected is a white powder, and the pass rate of the 0.1 mm square sieve is more than 90%.
  • the selected zinc dihydrogen phosphate is a white powder, and the pass rate of the 0.1 mm square sieve is more than 85%.
  • the selected urea is white powder, and the pass rate of 0.1mm square hole sieve is more than 85%.
  • the particle size of the temperature sensitive slow release antifreeze and deicing composite material for asphalt pavement is 0.1-6 mm.
  • the invention also provides a preparation method of the temperature sensitive slow release antifreeze and deicing composite material for the above asphalt pavement, the steps are as follows:
  • the chloride (and the rust inhibitor) is passed through a granulation and laminating machine to perform granulation to obtain core material particles;
  • the temperature sensitive agent is formulated into a solution, and the spray atomizing device is used to drive the compressed air as the power, and the temperature sensitive agent solution (using anhydrous organic solvent chloroform) is sprayed into a fog state to enter the coating device, and the temperature is foggy.
  • the sensitizer solution is in reverse contact with the core material particles obtained in the step (1), uniformly coated on the surface of the core material particles, and a uniform and dense polymer coating layer is formed on the surface of the core material particles, passing through (65-80) °C) heating dry solid film formation, cooling to obtain temperature sensitive slow release antifreeze deicing composite particles for asphalt pavement.
  • the surface of the core material forms a film layer with a certain thickness, and has a dense protective isolation at an ambient temperature higher than 0 ° C, and controls the dissolution of the core material.
  • this layer of controlled release film also has temperature sensitivity. When the ambient temperature is below 0 °C, this layer of dense protective film has a sustained release effect, so that the chloride is slowly released to the road surface, forming a salt layer and reducing the freezing point of the road surface.
  • the composite particles obtained above are sieved, dried, and conveyed to a silo through a belt, and the packaging workshop is fully packaged and packaged.
  • the process of infiltrating the temperature sensitive slow release type antifreeze and deicing composite particles in the present invention into the asphalt pavement is roughly: in the process of preparing the asphalt concrete for paving, the temperature sensitive slow release type antifreeze deicing according to the present invention Composite particles are added to it: In the asphalt concrete mixing production mixing tank, in the state of agitation, according to the order of size, fine material, straight material, mineral powder, asphalt, antifreeze and deicing materials (the proportion of antifreeze and deicing materials in asphalt concrete) 5-8%), the antifreeze deicing material is controlled to be discharged in the mixing tank for 40 seconds, and the white particles of the deicing antifreeze material are not seen in the mixed finished material, indicating that the antifreeze deicing material has been The asphalt is evenly wrapped around the belly.
  • the pavement construction process is similar to the conventional asphalt concrete construction process, and at the same time ensures that the pavement process porosity of the construction pavement is 3-5%.
  • the temperature-sensitive and slow-release anti-freeze deicing composite material with the rust inhibitor added in the invention is determined by the requirements of GB/T 18175 "Rotating and Hanging Method for Measuring Corrosion Inhibition Performance of Water Treatment Agent", due to the high-efficiency rust inhibitor Adding, the rust inhibitor component has a chemical property of forming a complex with a metal ion, and when in contact with the metal, forms a complex reaction equilibrium on the metal surface, forming a protective film to prevent the metal from being corroded, and effectively suppressing the metal being Chloride rust.
  • the components of these rust inhibitors are non-toxic, harmless, highly soluble, environmentally friendly and non-polluting.
  • the temperature-sensitive macromolecular material replaces the traditional slow-release material for coating, which not only can achieve the sustained release effect, but also makes the antifreeze material have a temperature-sensitive effect, overcoming the molecular heat of the chloride in the high temperature season.
  • the temperature-sensitive anti-freezing material can make the asphalt pavement achieve long-term anti-freezing effect, reduce the winter curing measures such as spreading the snow melting agent and using shoveling snow, and greatly reduce the maintenance cost of winter pavement management. At the same time, it ensures smooth roads in winter and reduces accidents.
  • Figure 1 is a flow chart showing the preparation process of the temperature sensitive slow release antifreeze and deicing composite material for asphalt pavement of the present invention
  • Figure 2 Comparison of corrosion rates of temperature-sensitive slow release antifreeze and deicing composites for asphalt pavement in Examples 1, 2 and 3.
  • the composition is 6% by weight of polyphenylene ether having a molecular weight of 2,000, 45% of polypropylene oxide having a molecular weight of 2000, and the balance being glycerol trilaurate.
  • the composition is 8% by weight of polyphenylene ether having a molecular weight of 2000, 50% of polypropylene oxide having a molecular weight of 2000, and the balance being glycerol trilaurate.
  • the preparation method is as shown in Example 1.
  • the preparation method is as shown in Example 1.
  • test results are expressed in terms of annual average corrosion depth in mm/a (take two test pieces as measurement results).
  • the temperature-sensitive sustained release antifreeze and deicing composite particles obtained in the above Examples 1, 2, 3 and 4 were completely dissolved in water to prepare a solution having a solute mass fraction of 18%.
  • the average value of the chloride ion concentration in the aqueous solution prepared by the four products in the first, second, third, and fourth embodiments, the chloride ion concentration is relatively close in the aqueous solution prepared by the four products, so
  • the design is to make the chloride ion concentration in the aqueous solution prepared by the product of the present invention in the three control solution solutions substantially the same, which is convenient for comparison)
  • the standard corrosion test piece is made of carbon steel No. 20 (GB/T 699) with a surface area of 28 cm 2 ;
  • Comparative Example 1 (chlorination mixture granulation) is prepared by weighing 75 g of sodium chloride and 15 g of calcium chloride, grinding the calcium chloride into a powder, and uniformly mixing with sodium chloride to obtain chlorine.
  • the granulation mixture is granulated by a granulating envelope integrated machine (the granulation process is the same as the granulation process in the step (1) of the above Example 2);
  • the calcium chloride is ground into a powder and mixed with sodium chloride to obtain a chloride mixture; the rust inhibitor is dissolved to prepare an aqueous solution having a solute mass fraction of 30%, and the aqueous solution of the rust inhibitor is sprayed on the chlorine by a metering pump.
  • granulation was carried out by means of a granulation envelope integrated machine (the granulation process was the same as the granulation process in the step (1) of the above Example 2).
  • the temperature-sensitive slow-release anti-freeze and de-icing composite material of the invention has strong hardness, can effectively prevent damage caused by the mixing process of the asphalt mixing tank, and breakage caused by the rolling of the gravity mechanical equipment in the road paving process.
  • the antifreeze and deicing composite material in the first embodiment of the present invention is blended into the asphalt mixture according to the mass percentage of 5-8%, and is uniformly dispersed, and is regarded as the asphalt mixture 1;
  • asphalt mixture 2 The asphalt mixture which is not incorporated into the antifreeze deicing composite material is counted as: asphalt mixture 2,
  • Asphalt mixture 1 and asphalt mixture 2 were prepared into rut test pieces 1 and 2, respectively, and water was sprinkled on the surface of the rut test piece, and then the test piece was placed in a low temperature incubator at -10 ° C for 8 h, and the test result was obtained. It indicates that the surface of the asphalt mixture surface to which the antifreeze deicing material is added is not frozen, and the surface layer of the asphalt mixture without the antifreeze deicing material has obvious ice layer;
  • the temperature of the cryostat is adjusted to -8 °C, -5 °C, -2 °C, and 0 °C to detect the rut test pieces 1 and 2 sprinkled on the surface. Whether the ice will freeze under the relevant temperature environment, the experimental procedure is the same as above. The results show that there is no ice on the surface of the asphalt mixture surface added with anti-freeze deicing materials, and the asphalt mixture surface layer without anti-freeze deicing material has obvious ice layer.
  • the experiment shows that the anti-freeze deicing material prepared by the invention has the effect of actively preventing the asphalt pavement from freezing at -10-0 °C.
  • Example 3 uncoated antifreeze material, ie, core material particles
  • uncoated antifreeze material ie, core material particles
  • the test of chloride release rate with a time span of 3 days was carried out at 20 ° C, 10 ° C, 0 ° C, and 10 ° C.
  • the experimental test results are as follows:
  • the chloride mass release rate in 3 days was the ratio of the mass of the chloride released by the antifreeze material in 3 days to the initial value.
  • the temperature-sensitive antifreeze material of the invention has obvious temperature-sensitive and sustained-release properties relative to the uncoated chloride core particles, and the temperature-sensitive coated chloride is at 10 to 30 ° C.
  • the release rate is much smaller than the uncoated chloride core particles; while at -10 to 0 °C, the temperature-sensitive coated chloride is normally released, and the release rate is substantially the same order of magnitude as the uncoated chloride particles. It has anti-freeze anti-knot function.

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Abstract

一种用于沥青路面的温敏型抗冻材料及其制备方法。该抗冻材料采用温敏型大分子有机物代替传统缓释剂，包膜在具有抗冻防结冰作用的氯化物颗粒表面，再通过筛分和干燥工艺而制成用于沥青路面温敏型抗冻材料。该抗冻材料能够根据外界的温度自动响应和控制抗冻材料中氯化物的释放温度，有效的增加氯化物在沥青路面中抗冻作用年限，延长抗冻材料的使用寿命。

Description

一种用于沥青路面的温敏型抗冻材料及其制备方法 技术领域
本发明属于道路路面防冻除冰技术领域，特别涉及一种用于沥青路面的温敏型抗冻材料及其制备方法。
背景技术
交通运输是国民经济的动脉，对整个国民经济发展起着不可估量的作用。随着我国经济的快速发展，公路交通已成为现代化城市的生命线。然而冬季冰雪致使车辆轮胎的附着系数大大降低，导致车祸频发和道路封锁，降低了道路的运输效率，同时造成了生命和财产损失。清除冬季道路冰雪，国内外均以被动技术为主包括使用机械和撒布融雪剂等，但是每年的人力和物力消耗巨大，难以大范围推广。
传统除冰雪的方法，主要是撒布融雪剂，或者采用机械为主、人工为辅的作业方法清除道路表面积雪，达到融雪抑冰的目的。但是这些措施在环保、机动、成本等方面都存在很大的局限性。为了方便、快捷、高效地除雪，主动除冰雪技术即在沥青混拌料中添加防冻除冰材料，该技术通过氯化物在沥青路面中起到降低路面冰点的作用，具有一次铺装，长期有效，维护成本低的特点，在欧洲和日本等发达地区已经得到广泛推广。
虽然现在人们已经可以在铺路过程中，成功地将氯化物加入到路面的沥青材料之中，但是由于沥青路面暴露在外，长期经受风吹雨打，特别是在高温季节时，沥青材料中的氯化物容易快速释放离开路面，这些都导致了路面中的氯化物利用率不高。
发明内容
本发明所要解决的技术问题在于：现有技术中，路面沥青材料中的氯化物，由于长期经受风吹雨打，特别是在高温季节时，氯化物容易快速释放离开路面，导致氯化物在道路防冻除冰方面的利用率不高。
为解决上述技术问题，本发明采用的技术方案是：
一种用于沥青路面的温敏型抗冻材料，即以氯化物为芯材，以温敏剂为包覆膜将芯材氯化物包覆在其中形成的颗粒状双层复合材料，
该复合材料的各组分按重量份数计算为，氯化物75-95份，温敏剂5-20份，
氯化物为氯化钠、氯化钙、氯化镁中一种或两种以上的混合物，
其中，温敏剂组成按重量百分比计算为，6—10％的分子量为2000的聚苯醚、40—55％的分子量为2000—6000的聚环氧丙烷，余量为甘油三月桂酸酯。
作为优选：上述沥青路面用的温敏缓释型防冻除冰复合材料中,还包括了缓蚀剂即阻锈剂，复合材料为，以氯化物和阻锈剂的混合物为芯材，以温敏剂作为包覆膜将氯化物和阻锈剂包覆在其中形成的颗粒状双层复合材料，
该复合材料的各组分按重量份数计算为，
氯化物75-95份、温敏剂5-20份。其六偏磷酸钠0.01-0.5份、葡萄糖酸钠0.01-0.5份、磷酸二氢锌0.01-0.5份、尿素0.01-0.5份；六偏磷酸钠、葡萄糖酸钠、磷酸二氢锌、尿素组成阻锈剂，
氯化物为氯化钠、氯化钙、氯化镁中一种或两种以上的混合物，
其中，所述的温敏剂组成按重量百分比计算为，6—10％的分子量为2000的聚苯醚、40—55％的分子量为2000—6000的聚环氧丙烷，余量为甘油三月桂酸酯。
选用的六偏磷酸钠为白色粉末，0.1mm方孔筛的通过率为大于85％以上，
选用的葡萄糖酸钠为白色粉末，0.1mm方孔筛的通过率为大于90％以上，
选用的磷酸二氢锌为白色粉末，0.1mm方孔筛的通过率为大于85％以上，
选用的尿素为白色粉末，0.1mm方孔筛的通过率为大于85％以上，
本发明中，沥青路面用的温敏缓释型防冻除冰复合材料颗粒的粒径大小为0.1—6mm。
本发明还提供了一种上述沥青路面用的温敏缓释型防冻除冰复合材料的制备方法，步骤为：
(1)先将氯化物(和阻锈剂)通过造粒包膜一体机设备，进行造粒，得到芯材颗粒；
(2)将温敏剂配成溶液，采用喷射雾化装置以压缩空气为动力，将温敏剂溶液(采用无水的有机溶剂氯仿，)喷射为雾态进入包膜设备中，雾状温敏剂溶液与步骤(1)中得到的芯材颗粒逆向接触，均匀地涂覆在芯材颗粒表面，在芯材颗粒表面形成一层均匀而致密的高分子包覆层，通过(65-80℃)加热干固成膜，冷却后得到沥青路面用的温敏缓释型防冻除冰复合材料颗粒。
包膜后芯材表面形成一定厚度的膜层，在环境温度高于0℃以上具有致密的保护隔离作用，控制芯材的溶解。另外这层控释衣膜还具有温敏性，当环境温度在0℃以下，这层致密保护膜，具有缓释作用，使得氯化物缓慢释放至路面，形成盐水层，降低路面的冰点。
将上述得到的复合材料颗粒筛分、干燥，通过皮带输送至料仓，包装车间全自动包装，封装。
将本发明中的温敏缓释型防冻除冰复合材料颗粒，渗入到沥青路面的过程大致为：在制备铺路用的沥青混泥土的过程中，将本发明的温敏缓释型防冻除冰复合材料颗粒加入其中： 在沥青混泥土拌合生产拌缸中，在搅拌状态下，按大小料、细料、直料、矿粉、沥青、防冻除冰材料的先后顺序添加(防冻除冰材料占沥青混泥土的比重为5-8％)，防冻除冰材料在拌缸的搅拌时间控制在40秒出料，在拌合好的成品料中看不到除冰防冻材料的白色颗粒，说明防冻除冰材料已被沥青均匀裹腹。
路面施工工艺与常规沥青混凝土施工工艺类似，同时保证施工路面摊铺工艺孔隙率为3-5％。
本发明的温敏缓释型防冻除冰复合材料的工作原理：
在沥青路面面层中添加温敏缓释型防冻除冰复合材料，受到来往行驶车辆的碾压和摩擦，利用了路面孔隙渗透压力和毛细管现象，使得防冻除冰复合材料从路面的不同深度渗透至路面附近，同时还具有低温缓慢释放氯化物效应。释放出的氯化物与路面冰雪接触，迅速溶于雪水中，随着雪水中氯化物离子浓度增加，水的液相蒸气压下降，而冰的固态蒸气压不变，为了达到冰水混合物固液蒸气压平衡的状态，冰便开始融化。从而可以防止和延缓冬季沥青路面结冰的现象。
本发明中添加有阻锈剂的温敏缓释型防冻除冰复合材料，通过GB/T 18175《水处理剂缓蚀性能的测定旋转挂片法》的要求进行测定，由于高效阻锈剂的添加，其阻锈剂组分具有与金属离子生成络合物的化学性质，在与金属接触时，在金属表面形成络合反应平衡，形成一层保护膜阻止金属被腐蚀，有效地抑制金属被氯化物锈蚀。另外这些阻锈剂的组分又具有无毒、无害、高溶解性的特性，对环境友好且无污染。
本发明的有益效果在于：
(1)具有温敏功能，温敏型大分子材料替代传统缓释材料进行包膜，不仅可以达到缓释的作用，使得抗冻材料具有温敏效应，克服氯化物在高温季节时由于分子热运动剧烈导致的大量无效释放问题，延长融雪沥青路面的使用年限；同时兼备低温时正常释放，沥青路面可以防止路面结冰的功能。
(2)具有抗冻温度可调功能，可以根据不同地区的冬季路面温度，调节和设计抗冻材料中氯化物组成，例如：—10℃以下地区可以适当增加芯材中氯化钙的组成，—10℃以上地区则可以适当增加芯材中氯化钠组成。
(3)具有缓释能力可调节功能，根据不同地区的降雨量和路面的湿度情况，通过调节温敏型大分子的分子量和包膜的厚度，减少高温季节时氯化物无效释放过快的问题。
(4)具有环保功能，高效阻锈剂的加入可以减少抗冻材料中的氯化物释放时对道路桥梁和行驶车辆的钢铁部件产生腐蚀作用，不会对环境造成不利影响。
(5)温敏型抗冻材料能使得沥青路面达到长久防结冻效果，减少撒播融雪剂和使用铲雪等冬季养护措施，大幅降低冬季路面管理养护成本。同时保证冬季道路畅通，降低意外事故的发生。
附图说明
图1：本发明的沥青路面用温敏缓释型防冻除冰复合材料的制备工艺流程图；
图2：实施例1、2、3中，沥青路面用温敏缓释型防冻除冰复合材料的腐蚀率测定对比图。
具体实施方式
实施例1
称取氯化钠80g、氯化钙10g、阻锈剂1g(六偏磷酸钠0.3g，葡萄糖酸钠0.2g、磷酸二氢锌0.2g和尿素0.3g)、温敏剂9g(温敏剂组成按重量百分比计算为，6％的分子量为2000的聚苯醚、45％的分子量为2000的聚环氧丙烷，余量为甘油三月桂酸酯)。
(1)将氯化钙磨成粉料，与氯化钠混合均匀，得到氯化物混合物；将阻锈剂溶解配制为溶质质量分数为30％的水溶液，通过计量泵将阻锈剂的水溶液喷撒在氯化物混合物中，一并通过造粒包膜一体机设备，进行造粒，得到粒径为2.5mm的芯材颗粒；
(2)采用喷射雾化装置以压缩空气为动力，将温敏剂溶液喷射为雾态进入包膜设备中，雾状温敏剂溶液与步骤(1)中得到的芯材颗粒逆向接触，均匀地涂覆在芯材颗粒表面，在芯材颗粒表面形成一层0.1mm均匀而致密的高分子包覆层，75℃加热1.5小时干固成膜，冷却后得到沥青路面用的温敏缓释型防冻除冰复合材料颗粒。
实施例2
称取氯化钠75g、氯化钙15g、(阻锈剂：六偏磷酸钠0.2g，葡萄糖酸钠0.3g、磷酸二氢锌0.2g和尿素0.3g)、温敏剂9g(温敏剂组成按重量百分比计算为，8％的分子量为2000的聚苯醚、50％的分子量为2000的聚环氧丙烷，余量为甘油三月桂酸酯)。
制备方法如实施例1所示。
实施例3
称取氯化钠盐80g、氯化钙15g、(阻锈剂：六偏磷酸钠0.2g，葡萄糖酸钠0.3g、磷酸二氢锌0.2g和尿素0.3g)、温敏剂14g(温敏剂组成按重量百分比计算为，6％的分子量为2000的聚苯醚、48％的分子量为2000的聚环氧丙烷，余量为甘油三月桂酸酯)。
制备方法如实施例1所示。
实施例4
称取氯化钠75g、氯化钙15g、温敏剂9g(温敏剂组成按重量百分比计算为，6％的分子量为2000的聚苯醚、45％的分子量为2000的聚环氧丙烷，余量为甘油三月桂酸酯)。
(1)将氯化钙磨成粉料，与氯化钠混合均匀，通过造粒包膜一体机设备，进行造粒，得到粒径为2.5mm的芯材颗粒；
(2)采用喷射雾化装置以压缩空气为动力，将温敏剂溶液喷射为雾态进入包膜设备中，雾状温敏剂溶液与步骤(1)中得到的芯材颗粒逆向接触，均匀地涂覆在芯材颗粒表面，在芯材颗粒表面形成一层0.1mm均匀而致密的高分子包覆层，75℃加热1.5小时干固成膜，冷却后得到沥青路面用的温敏缓释型防冻除冰复合材料颗粒。
实验1 本发明的温敏缓释型防冻除冰复合材料对碳钢的腐蚀率：
按照GB/T 18175的要求进行测定。测试结果以年平均腐蚀深度表示，单位mm/a(取两片试片作为测定结果)。
分别将上述实施例1、2、3、4中得到的温敏缓释型防冻除冰复合材料颗粒，完全溶解于水中，配成溶质质量分数为18％的溶液，
将纯水、氯化钠水溶液、氯化镁水溶液、氯化钙水溶液作为对照项，其中，氯化钠水溶液、氯化镁水溶液、氯化钙水溶液3者的氯离子浓度相同，且为实施例1、2、3、4中，四种产品配成的水溶液中氯离子浓度的平均值(实施例1、2、3、4中，四种产品配成的水溶液中，氯离子浓度是比较接近的，因此这样设计，是为了使这3个对照项溶液中，与本发明的产品配成的水溶液中，氯离子浓度基本持平，方便进行比较)，
测试条件：
(1)标准腐蚀试片采用20号碳钢(GB/T 699),表面积28cm2；
(2)溶液体积与试片面积比:24mL/cm2；
(3)测定温度40℃；
(4)测定周期48h；
(5)测定溶液中不通空气。
比较结果如表1：
表1：碳钢腐蚀率测定结果
Figure PCTCN2015089609-appb-000001
实验结果的坐标图如附图2所示(除实施例4溶液对应的数据)。由此得出高效阻锈剂的加入使得防冻除冰材料对碳钢腐蚀率大大降低，其指标优于国家标准GB/T23851-2009《道路除冰融雪剂》和北京市地方标准DB 11/T161-2012《融雪剂》。
实验2 本发明防冻除冰材料硬度测试
实验仪器：颗粒强度测定仪(日本藤原制作所制造)
测试步骤：
将颗粒强度测定仪调零，使指示杆在零点位置，随机抽取本发明中的温敏缓释型防冻除冰复合材料颗粒，将颗粒径向放于承受基座上，然后顺时针转动加力杆，此时在压力显示盘中压力指针会带着指示杆一同转动，当压力逐渐增大直至将颗粒压碎时，压力指示针回零，而压力指示杆停留的位置即为颗粒的强度，从实施例1、2、3中的颗粒样本中，随机取出10个颗粒(粒径大小在2.5—3mm)，按上述方法进行测定。舍弃一个最小值和一个最大值，其 余硬度值的平均值即为该防冻除冰材料的强度。测试结果如表2：
表2：防冻除冰剂硬度测试
Figure PCTCN2015089609-appb-000002
上表中“对比例1(氯化物混合物造粒)”的制备方法为：称取氯化钠75g和氯化钙15g，将氯化钙磨成粉料，与氯化钠混合均匀，得到氯化物混合物，通过造粒包膜一体机设备，进行造粒(造粒工艺与上述实施例2的步骤(1)中的造粒工艺相同)；
上表中“对比例2(氯化物、阻锈剂的混合物造粒)”的制备方法为：
称取氯化钠75g、氯化钙15g、(阻锈剂：六偏磷酸钠0.2g，葡萄糖酸钠0.3g、磷酸二氢锌0.2g和尿素0.3g)，
将氯化钙磨成粉料，与氯化钠混合均匀，得到氯化物混合物；将阻锈剂溶解配制为溶质质量分数为30％的水溶液，通过计量泵将阻锈剂的水溶液喷撒在氯化物混合物中，一并通过造粒包膜一体机设备，进行造粒(造粒工艺与上述实施例2的步骤(1)中的造粒工艺相同)。
从表2中(对比例1和对比例2的比较)的数据来看：阻锈剂的加入，对提高氯化物混合物颗粒的硬度是具有一定贡献的，但是贡献比较有限；同理，比较对比例1和实施例4之间的数据，可见采用温敏剂对氯化物混合物颗粒进行包覆，也能一定程度地提高复合材料的硬度，但是颗粒还是比较疏松。而只有当“加入阻锈剂”和“温敏剂包覆”这两个手段同时使用时，颗粒的硬度才大大提高，这是这两种改性手段起到的协同作用，因此“加入阻锈剂”不仅仅起到了抗腐蚀的作用，还有利于包覆颗粒硬度的提高。
本发明的温敏缓释型防冻除冰复合材料颗粒硬度强，可有效防止沥青拌缸搅拌过程中引起破损，以及路面摊铺工艺中重力机械设备碾压所引起的破碎。
实验3 本发明的温敏缓释型防冻除冰复合材料的路面除冰效果实验
将本发明实施例1中的防冻除冰复合材料，按质量百分数5—8％掺入到沥青混拌料中，分散均匀，计为沥青混拌料1；
将没有掺入防冻除冰复合材料的沥青混拌料计为：沥青混拌料2，
将沥青混拌料1、沥青混拌料2，分别制备成车辙试件1、2，分别在车辙试件表面撒水，然后把试件放在-10℃的低温恒温箱内冷冻8h，试验结果表明添加了防冻除冰材料的沥青混拌料面层表面没有结冰，未添加防冻除冰材料的沥青混拌料面层有明显冰层；
依次调整低温恒温箱内温度为-8℃、-5℃、-2℃、0℃，来检测表面撒水的车辙试件1、2，在相关温度环境下，是否会结冰，实验步骤同上。结果表明添加了防冻除冰材料的沥青混拌料面层表面均没有结冰，未添加防冻除冰材料的沥青混拌料面层均有明显冰层。
实验说明本发明制备的防冻除冰材料在-10-0℃时，具有主动防止沥青路面结冰效果。
实验4 本发明的防冻除冰复合材料在温敏缓释方面的效应
取实施例3中制备的包膜后和未包膜的抗冻材料(未包膜的抗冻材料即芯材颗粒)，参照HG/T3931-2007缓控释肥料的行业标准，在30℃、20℃、10℃、0℃、—10℃时进行时间跨度为3天的氯化物释放率的测试，实验测试结果如下：
表3
Figure PCTCN2015089609-appb-000003
其中3天内氯化物质量释放率为抗冻材料在3天内累计释放的氯化物质量与初始值之比。
分析以上实验数据可知，本发明的温敏型抗冻材料相对于未包膜的氯化物芯材颗粒，具有明显温敏缓释性能，在10～30℃时，温敏包覆的氯化物的释放速率远远小于未包膜的氯化物芯材颗粒；而在-10～0℃条件下，温敏包覆的氯化物正常释放，释放率基本与未包膜的氯化物颗粒处于同一数量级，具备防冻抗结的功能。

Claims (6)

  1. 一种用于沥青路面的温敏型抗冻材料，其特征在于：所述的复合材料为，以氯化物为芯材，以温敏剂为包覆膜的颗粒状双层复合材料，复合材料的各组分按重量份数计算为，氯化物75-95份，温敏剂5-20份，
    其中，所述的温敏剂组成按重量百分比计算为，6—10％的分子量为2000的聚苯醚、40—55％的分子量为2000—20000的聚环氧丙烷，余量为甘油三月桂酸酯。
  2. 一种用于沥青路面的温敏型抗冻材料，其特征在于：所述的复合材料为，以氯化物和阻锈剂的混合物为芯材，以温敏剂作为包覆膜的颗粒状双层复合材料，
    复合材料的各组分按重量份数计算为，氯化物75-95份、温敏剂5-20份、六偏磷酸钠0.01-0.5份、葡萄糖酸钠0.01-0.5份、磷酸二氢锌0.01-0.5份、尿素0.01-0.5份，
    其中，六偏磷酸钠、葡萄糖酸钠、磷酸二氢锌、尿素组成阻锈剂；
    所述的温敏剂组成按重量百分比计算为，6—10％的分子量为2000的聚苯醚、40—55％的分子量为2000—6000的聚环氧丙烷，余量为甘油三月桂酸酯。
  3. 如权利要求1或2所述的用于沥青路面的温敏型抗冻材料，其特征在于：所述的颗粒状双层复合材料的粒径大小为0.1—6mm。
  4. 如权利要求1或2所述的用于沥青路面的温敏型抗冻材料，其特征在于：所述的氯化物为氯化钠、氯化钙、氯化镁中一种或两种以上的混合物。
  5. 如权利要求1所述的用于沥青路面的温敏型抗冻材料的制备方法，其特征在于：所述制备方法的步骤为，
    (1)先将氯化物通过造粒包膜一体机设备，进行造粒，得到芯材颗粒；
    (2)将温敏剂配成溶液，采用喷射雾化装置以压缩空气为动力，将温敏剂溶液喷射为雾态进入包膜设备中，雾状温敏剂溶液与步骤(1)中得到的芯材颗粒逆向接触，均匀地涂覆在芯材颗粒表面，在芯材颗粒表面形成一层均匀而致密的高分子包覆层，通过加热干固成膜，冷却后得到用于沥青路面的温敏型抗冻材料颗粒。
  6. 如权利要求2所述的用于沥青路面的温敏型抗冻材料的制备方法，其特征在于：所述制备方法的步骤为，
    (1)先将氯化物和阻锈剂混合均匀，通过造粒包膜一体机设备，进行造粒，得到芯材颗粒；
    (2)将温敏剂配成溶液，采用喷射雾化装置以压缩空气为动力，将温敏剂溶液喷射为雾态进入包膜设备中，雾状温敏剂溶液与步骤(1)中得到的芯材颗粒逆向接触，均匀地涂覆在芯材颗粒表面，在芯材颗粒表面形成一层均匀而致密的高分子包覆层，通过加热干固成膜， 冷却后得到用于沥青路面的温敏型抗冻材料颗粒。
PCT/CN2015/089609 2015-04-10 2015-09-15 一种用于沥青路面的温敏型抗冻材料及其制备方法 WO2016161763A1 (zh)

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