CN107162069B - 一种三甲基丙酮酸合成工序中三氯化钌催化剂的回收工艺 - Google Patents
一种三甲基丙酮酸合成工序中三氯化钌催化剂的回收工艺 Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
本发明涉及化工行业三废处理技术领域,具体涉及一种三甲基丙酮酸合成工序中三氯化钌催化剂的回收工艺:将废三氯化钌催化剂加入溶液中加热搅拌,然后进行固液分离,滤液蒸发得到水合氯化钌,将水合氯化钌于氯化氢气体中保温处理即可,避免了碱熔法较大的能耗及废水生成量。将回收的无水三氯化钌与硅藻土复配后,可以直接用于三甲基丙酮酸制备工序。
Description
技术领域
本发明涉及化工行业三废处理技术领域,具体涉及一种三甲基丙酮酸合成工序中三氯化钌催化剂的回收工艺。
背景技术
嗪草酮是一种内吸性择性除草剂,药剂被杂草根系吸收随蒸腾流向上部传导,主要通过抑制敏感植物的光合作用发挥杀草活性,施药后各敏感杂草萌发出苗不受影响,出苗后叶片褪绿,最后营养枯竭而死。适用于大豆、马铃薯、番茄、甘蔗、玉米等田间作物多种阔叶杂草,也适用于某些禾本科杂草,对多年生杂草药效较差。
嗪草酮属于三嗪类除草剂中非均三嗪除草剂,活性高,持效期适中,现为万吨级旱田除草剂的骨干品种。嗪草酮最早由Bayer公司于1971年开发,此后美国Du Pont公司和Mobay Chemical Company公司也相继投入生产。嗪草酮的合成方法为:以三甲基丙酮酸和硫代卡巴肼为主要中间体,经环合、甲基化制得嗪草酮。
其中,三甲基丙酮酸的合成方法为:以频那酮为原料,经氯气氯化得二氯频那酮;二氯频那酮在氢氧化钠溶液中水解,进一步经次氯酸钠在催化剂的作用下,催化氧化得三甲基丙酮酸钠,酸化后得三甲基丙酮酸。该工序中使用的催化剂为硅藻土负载的无水三氯化钌,在反应过程中,负载三氯化钌催化剂吸水,失去催化活性,形成大量废固。
目前,国内回收三氯化钌的技术多为碱熔法,在焚烧和碱熔过程需要消耗大量能量,在碱熔-酸化浸出过程又产生大量含盐废水,增大了企业的生产和运营成本。
发明内容
本发明为了克服现有技术的不足,提供了一种三甲基丙酮酸合成工序中三氯化钌催化剂的回收工艺,实现催化剂的循环利用,
本发明采用的技术方案为:
(1)将废三氯化钌催化剂加入盐酸与甲醇的混合溶液中加热搅拌,然后进行固液分离,重复上述操作1~3次,
废三氯化钌催化剂在加入混合溶液之前经过了干燥、粉碎、经50~100目筛的预处理,
盐酸与甲醇的混合溶液中,盐酸和甲醇的质量比为0.5~2:1,其中盐酸的溶质质量分数为30%,
加热搅拌具体为在40~60℃下搅拌2~5小时;
(2)将步骤(1)中固液分离后得到的滤液蒸发回收盐酸-甲醇混合溶液,并得到水合氯化钌;
(3)将步骤(2)中得到的水合氯化钌干燥后于氯化氢气体中保温处理,得无水三氯化钌,
其中,干燥在40~50℃及绝对压力≤10Pa的真空环境下进行,干燥时间为3~5小时,
在氯化氢气体中于80~100℃保温处理5~8小时,氯化氢气体的流速为5~10立方米/小时,
对于三氯化钌而言,由于其水合物要转化为无水三氯化钌就必然会生成一羟基氯化钌和二羟基氯化钌化合物,而本发明中采用氯化氢气体与之反应取代其中的羟基得到无水的三氯化钌及副产物水,化学反应式如下:
RnCl2(OH)+HCl→RnClg+H2O
RnCl(OH)2+2HCl→RnClg+2H2O。
本发明的有益效果在于:使用物理萃提法分离三氯化钌与载体,避免了灼烧和碱熔工艺较大的能耗;萃提液通过二效蒸发器回收,可重复使用,无废水排放;将回收的无水三氯化钌与硅藻土复配后,可以直接用于三甲基丙酮酸的制备工序。
附图说明
图1为本发明的废催化剂回收工艺流程简图。
具体实施方式
实施例1
将干燥、粉碎、过50目筛后的废三氯化钌催化剂100克,加入1000克盐酸与甲醇的混合溶液(盐酸和甲醇的质量比为1:1,其中盐酸的溶质质量分数为30%)中,40℃搅拌5小时,离心机进行固液分离;
上述离心滤液通过二效石墨蒸发器蒸发回收盐酸-甲醇混合溶液,蒸发器内残留水合氯化钌;
将上述水合氯化钌在40℃及绝对压力10Pa下真空干燥5小时,体系恢复常压后,在流速为5立方米/小时的氯化氢气流保护下,80℃干燥8小时得回收无水三氯化钌。
取1克本实施例中的回收无水三氯化钌与100克硅藻土复配后,用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为95.3%。
对比实施例1a
取1克市售无水三氯化钌(纯度≥99%),按照实施例1的操作与100克硅藻土复配并用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为95.8%。
对比实施例1b
回收工艺中未进行氯化氢气体处理,其余原料、操作均同实施例1:
将干燥、粉碎、过50目筛后的废三氯化钌催化剂100克,加入1000克盐酸与甲醇的混合溶液(盐酸和甲醇的质量比为1:1,其中盐酸的溶质质量分数为30%)中,40℃搅拌5小时,离心机进行固液分离;
上述离心滤液通过二效石墨蒸发器蒸发回收盐酸-甲醇混合溶液,蒸发器内残留水合氯化钌;
将上述水合氯化钌在40℃及绝对压力10Pa下真空干燥5小时,体系恢复常压后,在80℃干燥8小时得回收三氯化钌。
取1克本对比实施例中的回收无水三氯化钌,按照实施例1的操作与100克硅藻土复配并用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为48.5%。
实施例2
将干燥、粉碎、过80目筛后的废三氯化钌催化剂100克,加入500克盐酸与甲醇的混合溶液(盐酸和甲醇的质量比为1:1,其中盐酸的溶质质量分数为30%)中,50℃搅拌4小时,离心机进行固液分离;
上述离心滤液通过二效石墨蒸发器蒸发回收盐酸-甲醇混合溶液,蒸发器内残留水合氯化钌;
将上述水合氯化钌在45℃及绝对压力10Pa下真空干燥4小时,体系恢复常压后,在流速为8立方米/小时的氯化氢气流保护下,90℃干燥6小时得回收无水三氯化钌。
取5克本实施例中的回收无水三氯化钌与100克硅藻土复配后,用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为96.2%。
对比实施例2
取5克市售无水三氯化钌(纯度≥99%),按照实施例2的操作与100克硅藻土复配并用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为96%。
实施例3
将干燥、粉碎、过100目筛后的废三氯化钌催化剂100克,加入200克盐酸与甲醇的混合溶液(盐酸和甲醇的质量比为2:1,其中盐酸的溶质质量分数为30%)中,60℃搅拌2小时,离心机进行固液分离;
上述离心滤液通过二效石墨蒸发器蒸发回收盐酸-甲醇混合溶液,蒸发器内残留水合氯化钌;
将上述水合氯化钌在50℃及绝对压力10Pa下真空干燥3小时,体系恢复常压后,在流速为10立方米/小时的氯化氢气流保护下,100℃干燥5小时得回收无水三氯化钌。
取10克本实施例中的回收无水三氯化钌与100克硅藻土复配后,用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为97.5%。
对比实施例3
取10克市售无水三氯化钌(纯度≥99%),按照实施例3的操作与100克硅藻土复配并用于三甲基丙酮酸的催化氧化制备工序,三甲基丙酮酸收率为97.4%。
Claims (6)
1.一种三甲基丙酮酸合成工序中三氯化钌催化剂的回收工艺,其特征在于:所述回收工艺为,
(1)将废三氯化钌催化剂加入溶液中加热搅拌,然后进行固液分离;所述的溶液为盐酸与甲醇的混合溶液;
(2)将步骤(1)中固液分离后的滤液蒸发得到水合氯化钌;
(3)将步骤(2)中得到的水合氯化钌于氯化氢气体中保温处理,得无水三氯化钌。
2.如权利要求1所述的三氯化钌催化剂的回收工艺,其特征在于:步骤(1)中,废三氯化钌催化剂在加入溶液之前经过了干燥、粉碎、经50~100目筛的预处理。
3.如权利要求1所述的三氯化钌催化剂的回收工艺,其特征在于:所述的盐酸与甲醇的混合溶液中,盐酸和甲醇的质量比为0.5~2:1,所述盐酸的溶质质量分数为30%。
4.如权利要求1所述的三氯化钌催化剂的回收工艺,其特征在于:步骤(1)中所述的加热搅拌具体为在40~60℃下搅拌2~5小时。
5.如权利要求1所述的三氯化钌催化剂的回收工艺,其特征在于:步骤(3)中,在氯化氢气体中于80~100℃保温处理5~8小时,氯化氢气体的流速为5~10立方米/小时。
6.如权利要求1所述的三氯化钌催化剂的回收工艺,其特征在于:步骤(3)中,在进入氯化氢气体中保温处理之前,水合氯化钌先在40~50℃及绝对压力≤10Pa的真空环境下干燥3~5小时。
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