CN115041219A - 一种废料转化油品用催化剂的制备方法 - Google Patents
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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- C—CHEMISTRY; METALLURGY
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
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Abstract
本发明公开了一种废料转化油品用催化剂的制备方法,该方法是先制备高比表面的硅铝基质材料,再将活性组份分散其中,具有适宜的孔径分布和比表面积,有利于废料的催化裂解,从而获得更佳的产物分布,提高废料回收的经济价值。
Description
技术领域
本发明涉及一种废料转化油品用催化剂的制备方法,属于催化剂制备领域。
背景技术
废橡胶是固体废弃物的一种,其来源主要是废橡胶制品,即报废的轮胎、人力车胎、胶管、胶带、工业杂品等,另外一部分来自橡胶制品厂生产过程中产生的边角料和废品。
废橡胶的处理是当今人们面临的严重问题之一,为了满足不断提高的材料性能要求,橡胶朝着高强度,耐磨稳定和耐老化的方向发展,同时也造成了废弃后的橡胶长时间不能自然降解的问题,大量的废旧橡胶造成了比塑料污染(白色污染)更难处理的黑色污染,全世界每年有数百万吨废橡胶产生。
其中之一的处理方法为生产再生胶,但生产过程中会产生大量的含酚、氨类、磷废水和含二氧化硫、硫化氢的废气,因此国外已淘汰该工艺。
目前国外的解决方法主要有两种,其一是废橡胶在高温、高压和高浓度氧气的环境下燃烧产生热量,为需要蒸汽的工厂提供补充能源,其不足是投资大,不安全及成本高。其二是用物理方法将废橡胶磨成粉再利用,缺点是只能利用天然胶部分,仍有大量二次废物。
国外还曾研究过热分解含聚异戊二烯的高分子橡胶断链变成小分子石油气及燃料油,分解后的废渣变成炭黑产品,仍处于试验阶段。
CN1073591C公开了一种废轮胎制汽柴油和炭黑的方法及其装置,该方法是将废轮胎破碎后送入热裂解反应器内,同时通入氮气,水蒸气,燃烧废气等作为载气,升温至370-500℃,停留5-20分钟可获得汽、轻柴油及重柴油。
CN1869160A公开了一种废旧轮胎催化裂解制燃料油的方法,使用了裂解催化剂钡钛矿复合氧化物。
目前废橡胶的热裂解或催化裂解成为研究热点,但基本上仍处于实验室阶段,而且存在收率低,选择性差等问题,需选择合适的催化剂改善裂解产物。
发明内容
针对现有技术存在的一些问题,本发明的目的是提供一种废料转化油品催化剂的制备方法,该方法是先制备高比表面的硅铝基质材料,再将活性组份分散其中,具有适宜的孔径分布和比表面积,有利于橡胶废料的催化裂解,进而获得更佳的产物分布,提高废料回收的经济价值。
本发明所述制备方法其步骤具体如下:
(1)向硫酸铝溶液中加入稀硫酸,控制pH值小于2.0;
(2)向(1)中的溶液中缓慢加入水玻璃溶液,控制溶液温度小于20℃;
(3)将(2)中的溶液与偏铝酸钠、水玻璃溶液并流混合均匀,静置陈化,过滤洗涤;
(4)将(3)中滤饼重新打浆,加入Y型分子筛,浆液磨细后喷雾造粒,焙烧后洗涤干燥,即得标题物。
步骤(1)中硫酸铝溶液的浓度以Al2O3计为90±2g/L。
步骤(2)(3)中水玻璃溶液的浓度以SiO2计为60±2g/L。
步骤(2)中硫酸铝和水玻璃加入质量比为Al2O3:SiO2=(6-8):1。
步骤(3)中偏铝酸钠溶液的浓度以Al2O3计为100±2g/L,其与水玻璃的加入质量比为Al2O3:SiO2=(1-2):1。
步骤(4)中Y型分子筛的加入比例为10-20wt%。
通过以上步骤制成的最终产品比表面大于450m2/g,介孔孔径分布为15-30nm,孔容大于0.5ml/g。
本发明制备的催化剂用于废橡胶转化油品具有以下显著优势:
(1)作为一种活性催化剂,可以加快反应速度,降低反应温度,降低了橡胶废料裂解反应的苛刻度,降低了设备要求,利于该工艺的推广。
(2)全合成的硅铝基质材料,具有适宜的孔径分布和比表面积,有利于废塑料初步裂解后大分子的扩散和反应,通过控制硅铝材料的酸量和酸性,能够获得更优的裂解产物。
(3)喷雾造粒的催化剂颗粒,流动性好,控制合适的平均粒径,有利于废橡胶颗粒与其接触,充分快速的气化分解,减少过度裂解降低生焦。
具体实施方式:
下面将结合实施例对本发明进一步说明,需要说明的是以下所述的实施例仅仅是本发明的一部分实施例,并不意味着是对本发明范围的限制。
所用原材料均为工业级,取自青岛惠城环保科技股份有限公司。
废橡胶粉碎成1-5mm颗粒,取自青岛某鞋厂下脚料。
评价装置为自建,管式反应炉,橡胶颗粒在玻璃锥形加料器中加压后喷射进入,催化剂料高5cm,反应温度480℃,产品经冷凝收集后使用气相色谱进行分析化验。
实施例1
(1)向4000ml硫酸铝溶液(Al2O3=90.2g/L)中加入12wt%的稀硫酸,pH值1.8;
(2)向(1)中的溶液中缓慢加入1000ml水玻璃溶液(SiO2=60.5g/L),控制溶液温度小于20℃;
(3)将(2)中的溶液与1800ml偏铝酸钠、3000ml水玻璃溶液并流混合均匀,静置陈化,过滤洗涤;
(4)将(3)中滤饼重新打浆,加入88克Y型分子筛,浆液磨细后喷雾造粒,焙烧后洗涤干燥,记做CAT-1。
实施例2
(1)向4000ml硫酸铝溶液(Al2O3=90.2g/L)中加入12wt%的稀硫酸,pH值1.2;
(2)向(1)中的溶液中缓慢加入667ml水玻璃溶液(SiO2=60.5g/L),控制溶液温度小于20℃;
(3)将(2)中的溶液与1350ml偏铝酸钠、1500ml水玻璃溶液并流混合均匀,静置陈化,过滤洗涤;
(4)将(3)中滤饼重新打浆,加入100克Y型分子筛,浆液磨细后喷雾造粒,焙烧后洗涤干燥,记做CAT-2。
两种催化剂预老化后使用自建评价装置进行评价,其结果如下:
CAT-1 | CAT-2 | |
干气,wt% | 4.37 | 4.15 |
液化气,wt% | 9.68 | 10.11 |
C5汽油,wt% | 34.94 | 35.88 |
柴油,wt% | 15.87 | 14.76 |
重油,wt% | 3.89 | 3.33 |
焦炭,wt% | 31.25 | 31.77 |
轻收,wt% | 60.49 | 60.75 |
丙烯,wt% | 3.29 | 3.58 |
总丁烯,wt% | 4.86 | 5.01 |
异丁烯,wt% | 2.47 | 2.62 |
从以上两组评价数据可以看出,使用本发明的催化剂转化橡胶废料,获得了较好的产物分布,其产生的轻收可以进一步处理以获得更高的经济价值,生产的焦炭燃烧后产生热量,供应需要能量的工序,以达到全厂能量平衡的目的。
Claims (7)
1.一种废料转化油品用催化剂的制备方法,其具体制备步骤如下:
(1)向硫酸铝溶液中加入稀硫酸,控制pH值小于2.0;
(2)向(1)中的溶液中缓慢加入水玻璃溶液,控制溶液温度小于20℃;
(3)将(2)中的溶液与偏铝酸钠、水玻璃溶液并流混合均匀,静置陈化,过滤洗涤;
(4)将(3)中滤饼重新打浆,加入Y型分子筛,浆液磨细后喷雾造粒,焙烧后洗涤干燥,即得标题物。
2.根据权利要求1所述的制备方法,其特征在于步骤(1)中硫酸铝溶液的浓度以Al2O3计为90±2g/L。
3.根据权利要求1所述的制备方法,其特征在于步骤(2)(3)中水玻璃溶液的浓度以SiO2计为60±2g/L。
4.根据权利要求1所述的制备方法,其特征在于步骤(2)中硫酸铝和水玻璃加入质量比为Al2O3:SiO2=(6-8):1。
5.根据权利要求1所述的制备方法,其特征在于步骤(3)中偏铝酸钠溶液的浓度以Al2O3计为100±2g/L,其与水玻璃的加入质量比为Al2O3:SiO2=(1-2):1。
6.根据权利要求1所述的制备方法,其特征在于步骤(4)中Y型分子筛的加入比例为10-20wt%。
7.根据权利要求1所述的制备方法,其特征在于制成的标题物比表面大于450m2/g,介孔孔径分布为15-30nm,孔容大于0.5ml/g。
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