CN106117024A - 一种异戊醛的制备方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/002—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by dehydrogenation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/005—Mixtures of molecular sieves comprising at least one molecular sieve which is not an aluminosilicate zeolite, e.g. from groups B01J29/03 - B01J29/049 or B01J29/82 - B01J29/89
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/10—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing iron group metals, noble metals or copper
- B01J29/106—Y-type faujasite
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/10—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing iron group metals, noble metals or copper
- B01J29/12—Noble metals
- B01J29/126—Y-type faujasite
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/7215—Zeolite Beta
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates [SAPO compounds]
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Abstract
本发明公开了一种异戊醛的制备方法,包括如下步骤,加热异戊醇至汽化,然后加入催化剂进行高温脱氢反应,反应生成的气体经冷凝、分离后得到半成品异戊醛;取半成品异戊醛向其中加入氢氧化钠,振摇、静置分层后,弃去水层,过滤有机层,保留滤液,滤液中通入装氧化铝的吸附剂柱进行吸附处理,然后将吸附后的异戊醛进行精馏得到纯度可达99.9%的异戊醛。本发明采用上述方案,异戊醇转化率可达99.9%,得到异戊醛纯度可达99.9%,能耗低,可以降低制造成本,在保证转换率和纯度的前提下,对设备无腐蚀,污染少,安全性高。
Description
技术领域
本发明涉及化工合成技术领域,尤其涉及一种以异戊醇为起始原料制备异戊醛的方法。
背景技术
异戊醛是制造异戊酸的原料,合成香料的中间体,食品工业及制药工业中的原料。前国内异戊醛的生产主要是用硫酸、重铬酸于液相中将异戊醇氧化成异戊醛。但该方法存在着设备腐蚀严重,环境污染严重以及副反应多等缺点。
醇脱氢是制备醛、酮的一种主要方法。铜、锌、镍、铂、钯、铑等金属或其合金,对于醇的脱氢具有很好的活性和很高的选择性,但铂等贵金属价格昂贵,目前主要使用铜、锌等金属作为催化剂。
早期多使用粒、网、纤维等形状的铜或黄铜等合金作为催化剂进行脱氢,该类催化剂有以下缺点 :由于催化剂单位质量的活性表面积很小,催化剂活性很低,在低温下转化率 很低,要求在 400℃以上,而高温下,催化剂积炭失活速率快,需要重复再生。
目前主要采用催化脱氢法,公开号为 CN1566056A 的发明公开了一种用黄铜类催化剂对异戊醇进行气相催化脱氢反应制备异戊醛的方法,所述的黄酮类催化剂包括铜/锌合金、铜/锡合金或铜 /镍合金,催化脱氢的反应温度在 400~500℃,反应液经精馏后,转化率为 95~96%,选择性达99%。采用此法,虽然产率和转化率都较高,但是仍然存在能耗高,以及在高温下催化剂易粉化、结焦,再生困难等缺点,仍然不能满足异戊醛的工业化批量生产要求。
发明内容
本发明要解决的技术问题是针对现有技术的不足提供一种异戊醇转化率可达99.9%,得到异戊醛纯度可达99.9%,能耗低,可以降低制造成本,在保证转换率和纯度的前提下,对设备无腐蚀,污染少,安全性高的用异戊醇制备异
戊醛的方法。
本发明采用以下技术方案,一种异戊醛的制备方法,包括如下步骤,
a、加热异戊醇至汽化,然后加入催化剂进行高温脱氢反应,反应生成的气体经冷凝、分离后得到半成品异戊醛;
b、取半成品异戊醛向其中加入氢氧化钠,振摇、静置分层后 , 弃去水层,过滤有机层,保留滤液,滤液中通入装氧化铝的吸附剂柱进行吸附处理,然后将吸附后的异戊醛进行精馏得到纯度可达99.9%的异戊醛。
以下是本发明的进一步改进:
步骤a中所述催化剂的空速为0.8/h,所述异戊醇的进料速度为500ml/h,汽化温度为300℃,催化脱氢的反应温度为800℃。
进一步改进:
所述步骤 b中,滤液以 0.5-30 柱体积/小时的速度流经装有氧化铝的吸附剂柱。
进一步改进:
所述催化剂由以下重量份的物质组成,无定形硅铝50份,分子筛8份,α氧化铝8份,三氧化二硼20份,三氧化二铁15份,纳米氧化锌颗粒19份,氧化锆8份;
所述分子筛为 SAPO-11分子筛、β 沸石分子筛及Y型分子筛的混合物,所述SAPO-11分子筛、β 沸石分子筛及Y型分子筛的质量比为3:3:2;
所述SAPO-11分子筛的相对结晶度为 98%, 晶体粒径为 2.5μm;
所述Y型分子筛的相对结晶度 95%~ 110%,晶体粒径为 1.8μm;
所述纳米氧化锌颗粒的粒径为 100-20nm,长度为 80-30nm;
所述无定形硅铝含氧化硅 8wt%-50wt%,比表面积为 700-800m 2 /g, 孔容为1.6-1.8ml/g,孔直径 8-15nm ,所占的孔容占总孔容的 95%- 98%,红外总酸量为 0.30 -0.45mmol/g,中强酸量 / 红外总酸量为 0.56 -0.81,L 酸量 /B 酸量为 1.40 -2.30;
上述催化剂的制备方法包括如下步骤:
1)、将氯铂酸、硝酸钾和水混合均匀加入硝酸,调节浸渍液的 pH 值为 1-2,得到浸渍液;
2)、将上述重量份的无定形硅铝、分子筛、α氧化铝、三氧化二硼、三氧化二铁、纳米氧化锌颗粒、氧化锆的混合物加入到浸渍液中,得到浸渍处理的载体;
3)、浸渍处理后的载体,经升温干燥,焙烧,洗涤,然后干燥脱水,得到催化剂;
步骤1)中氯铂酸、硝酸钾和水的摩尔比为 1 :15:30000;
步骤2)中浸渍温度为 70-90℃,浸渍时间为3-8小时;
步骤3)中升温干燥条件为,以 2℃ /min 的速率升温至 400℃,停留 3-5小时 ;再以0.5℃ /min 的速率升温至 500℃,停留 8小时;
步骤3)中焙烧温度为 300-500℃,焙烧时间为 4-5小时;
步骤3)中干燥脱水的干燥温度 100-120℃,干燥时间为 4-6 小时。
本发明采用上述方案,异戊醇转化率可达99.9%,得到异戊醛纯度可达99.9%,能耗低,可以降低制造成本,在保证转换率和纯度的前提下,对设备无腐蚀,污染少,安全性高。
具体实施方式
实施例,一种异戊醛的制备方法,包括如下步骤,
a、加热异戊醇至汽化,然后加入催化剂进行高温脱氢反应,反应生成的气体经冷凝、分离后得到半成品异戊醛;
b、取半成品异戊醛向其中加入氢氧化钠,振摇、静置分层后 , 弃去水层,过滤有机层,保留滤液,滤液中通入装氧化铝的吸附剂柱进行吸附处理,然后将吸附后的异戊醛进行精馏得到纯度可达99.9%的异戊醛。
步骤a中所述催化剂的空速为0.8/h,所述异戊醇的进料速度为500ml/h,汽化温度为300℃,催化脱氢的反应温度为800℃。
所述步骤 b中,滤液以 0.5-30 柱体积/小时的速度流经装有氧化铝的吸附剂柱。
所述催化剂由以下重量份的物质组成,无定形硅铝50份,分子筛8份,α氧化铝8份,三氧化二硼20份,三氧化二铁15份,纳米氧化锌颗粒19份,氧化锆8份。
所述分子筛为 SAPO-11分子筛、β 沸石分子筛及Y型分子筛的混合物,所述SAPO-11分子筛、β 沸石分子筛及Y型分子筛的质量比为3:3:2。
所述SAPO-11分子筛的相对结晶度为 98%, 晶体粒径为 2.5μm。
所述Y型分子筛的相对结晶度 95%~ 110%,晶体粒径为 1.8μm。
所述纳米氧化锌颗粒的粒径为 100-20nm,长度为 80-30nm。
所述无定形硅铝含氧化硅 8wt%-50wt%,比表面积为 700-800m 2 /g, 孔容为1.6-1.8ml/g,孔直径 8-15nm ,所占的孔容占总孔容的 95%- 98%,红外总酸量为 0.30- 0.45mmol/g,中强酸量 / 红外总酸量为 0.56 -0.81,L 酸量 /B 酸量为 1.40 -2.30。
上述SAPO-11分子筛、Y型分子筛、纳米氧化锌颗粒及无定形硅铝的制备方法采用本领域常规制备方法,本发明不在详述。
上述催化剂的制备方法包括如下步骤:
1)、将氯铂酸、硝酸钾和水混合均匀加入硝酸,调节浸渍液的 pH 值为 1-2,得到浸渍液;
2)、将上述重量份的无定形硅铝、分子筛、α氧化铝、三氧化二硼、三氧化二铁、纳米氧化锌颗粒、氧化锆的混合物加入到浸渍液中,得到浸渍处理的载体;
3)、浸渍处理后的载体,经升温干燥,焙烧,洗涤,然后干燥脱水,得到催化剂。
步骤1)中氯铂酸、硝酸钾和水的摩尔比为 1 :15:30000。
步骤2)中浸渍温度为 70-90℃,浸渍时间为3-8小时。
步骤3)中升温干燥条件为,以 2℃ /min 的速率升温至 400℃,停留 3-5小时 ;再以 0.5℃ /min 的速率升温至 500℃,停留 8小时。
步骤3)中焙烧温度为 300-500℃,焙烧时间为 4-5小时。
步骤3)中干燥脱水的干燥温度 100-120℃,干燥时间为 4-6 小时。
Claims (4)
1.一种异戊醛的制备方法,其特征在于:包括如下步骤,
a、加热异戊醇至汽化,然后加入催化剂进行高温脱氢反应,反应生成的气体经冷凝、分离后得到半成品异戊醛;
b、取半成品异戊醛向其中加入氢氧化钠,振摇、静置分层后 , 弃去水层,过滤有机层,保留滤液,滤液中通入装氧化铝的吸附剂柱进行吸附处理,然后将吸附后的异戊醛进行精馏得到纯度可达99.9%的异戊醛。
2.根据权利要求1所述的异戊醛的制备方法,其特征在于:步骤a中所述催化剂的空速为0.8/h,所述异戊醇的进料速度为500ml/h,汽化温度为300℃,催化脱氢的反应温度为800℃。
3.根据权利要求1所述的异戊醛的制备方法,其特征在于:所述步骤 b中,滤液以 0.5-30 柱体积/小时的速度流经装有氧化铝的吸附剂柱。
4.根据权利要求1所述的异戊醛的制备方法,其特征在于:所述催化剂由以下重量份的物质组成,无定形硅铝50份,分子筛8份,α氧化铝8份,三氧化二硼20份,三氧化二铁15份,纳米氧化锌颗粒19份,氧化锆8份;
所述分子筛为 SAPO-11分子筛、β 沸石分子筛及Y型分子筛的混合物,所述SAPO-11分子筛、β 沸石分子筛及Y型分子筛的质量比为3:3:2;
所述SAPO-11分子筛的相对结晶度为 98%, 晶体粒径为 2.5μm;
所述Y型分子筛的相对结晶度 95%~ 110%,晶体粒径为 1.8μm;
所述纳米氧化锌颗粒的粒径为 100-20nm,长度为 80-30nm;
所述无定形硅铝含氧化硅 8wt%-50wt%,比表面积为 700-800m 2 /g, 孔容为1.6-1.8ml/g,孔直径 8-15nm ,所占的孔容占总孔容的 95%- 98%,红外总酸量为 0.30 -0.45mmol/g,中强酸量 / 红外总酸量为 0.56 -0.81,L 酸量 /B 酸量为 1.40 -2.30;
上述催化剂的制备方法包括如下步骤:
1)、将氯铂酸、硝酸钾和水混合均匀加入硝酸,调节浸渍液的 pH 值为 1-2,得到浸渍液;
2)、将上述重量份的无定形硅铝、分子筛、α氧化铝、三氧化二硼、三氧化二铁、纳米氧化锌颗粒、氧化锆的混合物加入到浸渍液中,得到浸渍处理的载体;
3)、浸渍处理后的载体,经升温干燥,焙烧,洗涤,然后干燥脱水,得到催化剂;
步骤1)中氯铂酸、硝酸钾和水的摩尔比为 1 :15:30000;
步骤2)中浸渍温度为 70-90℃,浸渍时间为3-8小时;
步骤3)中升温干燥条件为,以 2℃ /min 的速率升温至 400℃,停留 3-5小时 ;再以0.5℃ /min 的速率升温至 500℃,停留 8小时;
步骤3)中焙烧温度为 300-500℃,焙烧时间为 4-5小时;
步骤3)中干燥脱水的干燥温度 100-120℃,干燥时间为 4-6 小时。
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