CN111269360A - A kind of waste rubber powder polymerization grafting modification process of methyl methacrylate - Google Patents
A kind of waste rubber powder polymerization grafting modification process of methyl methacrylate Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000012986 modification Methods 0.000 title claims abstract description 17
- 230000004048 modification Effects 0.000 title claims abstract description 17
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 7
- 239000002699 waste material Substances 0.000 title claims abstract description 7
- 239000010426 asphalt Substances 0.000 claims abstract description 54
- 239000010920 waste tyre Substances 0.000 claims abstract description 33
- 239000003607 modifier Substances 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims 2
- 238000000227 grinding Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 230000035515 penetration Effects 0.000 abstract description 14
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 4
- 239000004926 polymethyl methacrylate Substances 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
- C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F253/00—Macromolecular compounds obtained by polymerising monomers on to natural rubbers or derivatives thereof
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- 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
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Abstract
本发明涉及一种废胶粉的甲基丙烯酸甲酯聚合接枝改性工艺，具体步骤包括：将废轮胎胶粉分散在水中，加入一定量的引发剂和表面改性剂，恒温搅拌1‑12小时，温度为50‑90℃，引发剂用量占胶粉质量的1.7％‑10％，表面改性剂用量为胶粉质量的1％‑300％。将接枝胶粉作为沥青改性剂通过湿法改性工艺制备胶粉改性沥青，以调控改性沥青性能。该方法操作简单，成本低廉，并且能够有效调控胶粉改性沥青的针入度、延度、软化点等主要性能。The invention relates to a methyl methacrylate polymerization grafting modification process for waste rubber powder. The specific steps include: dispersing waste tire rubber powder in water, adding a certain amount of initiator and surface modifier, and stirring at a constant temperature for 1-1 12 hours, the temperature is 50-90°C, the amount of initiator is 1.7%-10% of the mass of the rubber powder, and the amount of the surface modifier is 1%-300% of the mass of the rubber powder. The grafted rubber powder was used as the asphalt modifier to prepare the rubber powder modified asphalt through the wet modification process to control the performance of the modified asphalt. The method has simple operation and low cost, and can effectively control the main properties such as penetration, ductility and softening point of the rubber powder modified asphalt.
Description
技术领域technical field
本发明涉及一种废胶粉的甲基丙烯酸甲酯聚合接枝改性工艺。具体地说是采用聚合接枝的方法将聚甲基丙烯酸甲酯接枝到废轮胎胶粉表面，以调控胶粉改性沥青性能的工艺技术。The invention relates to a methyl methacrylate polymerization graft modification process of waste rubber powder. Specifically, it is a process technology of grafting polymethyl methacrylate to the surface of waste tire rubber powder by the method of polymerization grafting to regulate the performance of rubber powder modified asphalt.
背景技术Background technique
随着我国汽车行业的快速发展及家用轿车数量的快速增长，我国每年产生的废旧轮胎正以8％-10％的速度急剧增加，已是全球废旧轮胎产量最高的国家。预计到2020年，我国废轮胎产生量将达2000万吨。废轮胎成分复杂且不易降解，大量堆积不仅占用土地资源，也会造成环境污染。而我国橡胶消耗量大，橡胶资源匮乏，因此，提高对废旧轮胎资源的综合利用率成为一个亟待解决的课题。With the rapid development of my country's automobile industry and the rapid growth of the number of family cars, my country's annual waste tires are increasing sharply at a rate of 8%-10%, and it is already the country with the highest output of waste tires in the world. It is estimated that by 2020, my country's waste tire production will reach 20 million tons. The composition of waste tires is complex and difficult to degrade, and a large amount of accumulation not only occupies land resources, but also causes environmental pollution. However, my country's rubber consumption is large and rubber resources are scarce. Therefore, improving the comprehensive utilization rate of waste tire resources has become an urgent issue to be solved.
将石油沥青用作道路铺装材料有着悠久的历史，但是随着交通运输量的增大，人们对于路面性能提出了更高的要求。研究表明，沥青中掺入废轮胎胶粉进行改性，可以大批量消耗废旧轮胎，减轻废轮胎堆积对环境造成的压力；能够提高沥青的高温稳定性、低温抗裂性、抗老化和耐久性，并且能够有效降低路面噪音，减少路面反光，提高路面防滑效果，引起了人们的普遍关注。同时用废轮胎胶粉替换高成本的SBS 沥青改性剂，减少铺路成本，因此道路修筑采用胶粉改性沥青极具发展潜力。但由于胶粉与沥青相容性差等因素，限制了胶粉改性沥青的应用。通过将聚甲基丙烯酸甲酯接枝到废轮胎胶粉表面，能够在胶粉与沥青之间形成类似于SBS改性沥青的表面网状结构，从而提高胶粉改性沥青的性能。The use of petroleum asphalt as a road pavement has a long history, but with the increase in traffic, people put forward higher requirements for pavement performance. Studies have shown that mixing waste tire rubber powder into asphalt for modification can consume waste tires in large quantities and reduce the pressure on the environment caused by the accumulation of waste tires; it can improve the high temperature stability, low temperature crack resistance, aging resistance and durability of asphalt. , and can effectively reduce road noise, reduce road reflection, and improve the anti-skid effect of the road, which has attracted widespread attention. At the same time, the high-cost SBS asphalt modifier is replaced with waste tire rubber powder to reduce the cost of paving. Therefore, the use of rubber powder modified asphalt for road construction has great potential for development. However, due to factors such as poor compatibility between rubber powder and asphalt, the application of rubber powder modified asphalt is limited. By grafting polymethyl methacrylate onto the surface of waste tire rubber powder, a surface network structure similar to SBS modified asphalt can be formed between the rubber powder and the asphalt, thereby improving the performance of the rubber powder modified asphalt.
发明内容SUMMARY OF THE INVENTION
本发明提供一种简便、易于工业应用的废胶粉的甲基丙烯酸甲酯聚合接枝改性工艺。The invention provides a simple and easy industrial application of a methyl methacrylate polymerization graft modification process of waste rubber powder.
本发明采用的技术方案为：废轮胎胶粉分散在水中，加入一定量的引发剂和表面改性剂，恒温搅拌1-12 小时，温度为50-90℃，引发剂用量占胶粉质量的1.7％-10％，表面改性剂用量为胶粉质量的1％-300％。反应结束后，将废轮胎胶粉抽滤、洗涤、烘干、称重，测得质量接枝率，制得接枝胶粉。将接枝胶粉通过湿法改性工艺制备胶粉改性沥青，并检测其主要性能指标。The technical scheme adopted in the present invention is as follows: waste tire rubber powder is dispersed in water, a certain amount of initiator and surface modifier are added, constant temperature stirring is performed for 1-12 hours, the temperature is 50-90° C., and the amount of the initiator accounts for 50% of the mass of the rubber powder. 1.7%-10%, and the amount of surface modifier is 1%-300% of the quality of the rubber powder. After the reaction is completed, the waste tire rubber powder is suction filtered, washed, dried and weighed, and the mass grafting rate is measured to obtain the grafted rubber powder. The grafted rubber powder was prepared by wet modification process to prepare rubber powder modified asphalt, and its main performance indicators were tested.
所述引发剂为过氧苯甲酰，用量为苯乙烯用量的1.7％-10％。The initiator is benzoyl peroxide, and the dosage is 1.7%-10% of the amount of styrene.
所述表面改性剂为甲基丙烯酸甲酯，用量为胶粉质量的1％-300％。The surface modifier is methyl methacrylate, and the dosage is 1%-300% of the mass of the rubber powder.
所述反应温度为50-90℃。The reaction temperature is 50-90°C.
所述质量接枝率＝(接枝后胶粉质量-接枝前胶粉质量)/接枝前胶粉质量。The mass graft ratio=(quality of rubber powder after grafting-quality of rubber powder before grafting)/quality of rubber powder before grafting.
所述废轮胎胶粉的粒径为40目，胶粉来源为废轮胎粉碎。The particle size of the waste tire rubber powder is 40 meshes, and the source of the rubber powder is the crushing of waste tires.
所述反应时间为1-12小时。The reaction time is 1-12 hours.
所述基质沥青为道路沥青。The base asphalt is road asphalt.
所述废轮胎胶粉改性沥青湿法改性工艺的技术流程图见图。The technical flow chart of the waste tire rubber powder modified asphalt wet modification process is shown in the figure.
所述沥青主要性能指标包括25℃针入度、5℃延度、软化点。25℃针入度是表示沥青软硬程度和稠度、抵抗剪切破坏的能力，反映在一定条件下沥青的相对黏度的指标。5℃延度表示沥青抗张拉强度，延度越大，低温性能越好；软化点表示高温稳定性能，软化点越大，高温稳定性能越好。The main performance indicators of the asphalt include penetration at 25°C, ductility at 5°C, and softening point. Penetration at 25°C is an index that expresses the degree of softness, hardness and consistency of asphalt, and the ability to resist shear damage, and reflects the relative viscosity of asphalt under certain conditions. The ductility at 5°C represents the tensile strength of asphalt, the greater the ductility, the better the low temperature performance; the softening point represents the high temperature stability performance, the larger the softening point, the better the high temperature stability performance.
本发明具有如下优点：The present invention has the following advantages:
1.通过聚合接枝的方法实现对废轮胎胶粉的表面改性。采用甲基丙烯酸甲酯为接枝单体，过氧化苯甲酰为引发剂，在一定温度下将聚甲基丙烯酸甲酯接枝到废轮胎胶粉表面。将接枝后的胶粉应用于改性沥青，可使胶粉与沥青之间形成类似于SBS改性沥青的表面网状结构，使胶粉与沥青稳定相容，从而提高改性沥青的性能和稳定性。1. The surface modification of waste tire rubber powder is realized by the method of polymerization and grafting. Using methyl methacrylate as the grafting monomer and benzoyl peroxide as the initiator, the polymethyl methacrylate is grafted to the surface of the waste tire rubber powder at a certain temperature. Applying the grafted rubber powder to the modified asphalt can form a surface network structure similar to the SBS modified asphalt between the rubber powder and the asphalt, so that the rubber powder and the asphalt are stably compatible, thereby improving the performance of the modified asphalt and stability.
2.调控胶粉改性沥青的性能指标。通过在胶粉表面接枝不同量的聚甲基丙烯酸甲酯链段，调控胶粉与沥青的相容性，从而实现改性沥青25℃针入度、5℃延度和软化点的调控。2. Regulate the performance index of rubber powder modified asphalt. By grafting different amounts of polymethyl methacrylate segments on the surface of the rubber powder, the compatibility of the rubber powder and the asphalt is regulated, so as to realize the regulation of the 25°C penetration, 5°C ductility and softening point of the modified asphalt.
3.易于操作和工业化应用。本发明所采用的处理工艺简单，成本低廉，易于操作，可实现工业化应用。3. Easy to operate and industrialized application. The processing technology adopted by the invention is simple, the cost is low, the operation is easy, and the industrial application can be realized.
附图说明Description of drawings
图1是湿法改性工艺图。Fig. 1 is a wet modification process diagram.
具体实施方式Detailed ways
下面通过实施例进一步描述本发明的特征，但本发明并不局限于下述实例。The features of the present invention are further described below by means of examples, but the present invention is not limited to the following examples.
实施例1Example 1
将100g废轮胎胶粉、5g过氧化苯甲酰和300mL甲基丙烯酸甲酯分散于400mL水中，在60℃恒温搅拌下反应12小时。对反应后的废轮胎胶粉进行过滤、洗涤，80℃烘干至质量恒定，制得改性胶粉。测得胶粉质量接枝率为58％。将改性胶粉与70号基质沥青通过湿法改性工艺制备胶粉改性沥青，测定改性沥青的25℃针入度、5℃延度和软化点。测得25℃针入度为42(0.1mm)，5℃延度为7.6(cm)，软化点为67.4(℃)。Disperse 100 g of waste tire rubber powder, 5 g of benzoyl peroxide and 300 mL of methyl methacrylate in 400 mL of water, and react at a constant temperature of 60°C for 12 hours with stirring. The reacted waste tire rubber powder is filtered, washed, and dried at 80°C until the quality is constant to obtain modified rubber powder. The grafting ratio of rubber powder was measured to be 58%. Modified rubber powder and No. 70 base asphalt were prepared by wet modification process to prepare rubber powder modified asphalt, and the 25 ℃ penetration, 5 ℃ ductility and softening point of the modified asphalt were measured. The penetration at 25°C was measured to be 42 (0.1 mm), the ductility at 5°C was 7.6 (cm), and the softening point was 67.4 (°C).
实施例2Example 2
将100g废轮胎胶粉、5g过氧化苯甲酰和300mL甲基丙烯酸甲酯分散于400mL水中，在60℃恒温搅拌下反应2小时。对反应后的废轮胎胶粉进行过滤、洗涤，80℃烘干至质量恒定，制得改性胶粉。测得胶粉质量接枝率为10％。将改性胶粉与70号基质沥青通过湿法改性工艺制备胶粉改性沥青，定改性沥青的 25℃针入度、5℃延度和软化点。测得25℃针入度为42(0.1mm)，5℃延度为7.8(cm)，软化点为67.2(℃)。Disperse 100 g of waste tire rubber powder, 5 g of benzoyl peroxide and 300 mL of methyl methacrylate in 400 mL of water, and react at a constant temperature of 60°C for 2 hours with stirring. The reacted waste tire rubber powder is filtered, washed, and dried at 80°C until the quality is constant to obtain modified rubber powder. The grafting ratio of rubber powder mass was measured to be 10%. Modified rubber powder and No. 70 base asphalt were prepared by wet modification process to prepare rubber powder modified asphalt, and the 25°C penetration, 5°C ductility and softening point of the modified asphalt were determined. The penetration at 25°C was measured to be 42 (0.1 mm), the ductility at 5°C was 7.8 (cm), and the softening point was 67.2 (°C).
实施例3Example 3
将100g废轮胎胶粉、5g过氧化苯甲酰和300mL甲基丙烯酸甲酯分散于400mL水中，在60℃恒温搅拌下反应6小时。对反应后的废轮胎胶粉进行过滤、洗涤，80℃烘干至质量恒定，制得改性胶粉。测得胶粉质量接枝率为22％。将改性胶粉与70号基质沥青通过湿法改性工艺制备胶粉改性沥青，测定改性沥青的25℃针入度、5℃延度和软化点。测得25℃针入度为45(0.1mm)，5℃延度为8.6(cm)，软化点为66.2(℃)。Disperse 100 g of waste tire rubber powder, 5 g of benzoyl peroxide and 300 mL of methyl methacrylate in 400 mL of water, and react at a constant temperature of 60° C. for 6 hours with stirring. The reacted waste tire rubber powder is filtered, washed, and dried at 80°C until the quality is constant to obtain modified rubber powder. The grafting ratio of rubber powder was measured to be 22%. Modified rubber powder and No. 70 base asphalt were prepared by wet modification process to prepare rubber powder modified asphalt, and the 25 ℃ penetration, 5 ℃ ductility and softening point of the modified asphalt were measured. The penetration at 25°C was measured to be 45 (0.1 mm), the ductility at 5°C was 8.6 (cm), and the softening point was 66.2 (°C).
实施例4Example 4
将100g废轮胎胶粉、5g过氧化苯甲酰和100mL甲基丙烯酸甲酯分散于400mL水中，在60℃恒温搅拌下反应8小时。对反应后的废轮胎胶粉进行过滤、洗涤，80℃烘干至质量恒定，制得改性胶粉。测得胶粉质量接枝率为33％。将改性胶粉与70号基质沥青通过湿法改性工艺制备胶粉改性沥青，测定改性沥青的25℃针入度、5℃延度和软化点。测得25℃针入度为48(0.1mm)，5℃延度为8.8(cm)，软化点为64.8(℃)。Disperse 100 g of waste tire rubber powder, 5 g of benzoyl peroxide and 100 mL of methyl methacrylate in 400 mL of water, and react under constant stirring at 60° C. for 8 hours. The reacted waste tire rubber powder is filtered, washed, and dried at 80°C until the quality is constant to obtain modified rubber powder. The grafting ratio of rubber powder mass was measured to be 33%. Modified rubber powder and No. 70 base asphalt were prepared by wet modification process to prepare rubber powder modified asphalt, and the 25 ℃ penetration, 5 ℃ ductility and softening point of the modified asphalt were measured. The penetration at 25°C was measured to be 48 (0.1 mm), the ductility at 5°C was 8.8 (cm), and the softening point was 64.8 (°C).
实施例5Example 5
将100g废轮胎胶粉、5g过氧化苯甲酰和200mL甲基丙烯酸甲酯分散于400mL水中，在60℃恒温搅拌下反应8小时。对反应后的废轮胎胶粉进行过滤、洗涤，80℃烘干至质量恒定，制得改性胶粉。测得胶粉质量接枝率为31％。将改性胶粉与70号基质沥青通过湿法改性工艺制备胶粉改性沥青，测定改性沥青的25℃针入度、5℃延度和软化点。测得25℃针入度为47(0.1mm)，5℃延度为8.7(cm)，软化点为65.5(℃)。Disperse 100 g of waste tire rubber powder, 5 g of benzoyl peroxide and 200 mL of methyl methacrylate in 400 mL of water, and react at a constant temperature of 60° C. for 8 hours with stirring. The reacted waste tire rubber powder is filtered, washed, and dried at 80°C until the quality is constant to obtain modified rubber powder. The grafting ratio of rubber powder was measured to be 31%. Modified rubber powder and No. 70 base asphalt were prepared by wet modification process to prepare rubber powder modified asphalt, and the 25 ℃ penetration, 5 ℃ ductility and softening point of the modified asphalt were measured. The penetration at 25°C was measured to be 47 (0.1 mm), the ductility at 5°C was 8.7 (cm), and the softening point was 65.5 (°C).
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| CN111704757A (en) * | 2020-07-03 | 2020-09-25 | 苏州科技大学 | A kind of preparation method and application of semi-interpenetrating network structure polybutyl acrylate/waste tire rubber powder |
| CN115322583A (en) * | 2022-09-26 | 2022-11-11 | 厦门新立基股份有限公司 | High-viscosity high-elasticity modified asphalt mixture and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704757A (en) * | 2020-07-03 | 2020-09-25 | 苏州科技大学 | A kind of preparation method and application of semi-interpenetrating network structure polybutyl acrylate/waste tire rubber powder |
| CN111704757B (en) * | 2020-07-03 | 2022-04-15 | 苏州科技大学 | Preparation method and application of semi-interpenetrating network structure polybutyl acrylate/waste tire rubber powder |
| CN115322583A (en) * | 2022-09-26 | 2022-11-11 | 厦门新立基股份有限公司 | High-viscosity high-elasticity modified asphalt mixture and preparation method thereof |
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Application publication date: 20200612 |