CN111085270A - Preparation method of ammonium octamolybdate-based supramolecular material catalyst - Google Patents
Preparation method of ammonium octamolybdate-based supramolecular material catalyst Download PDFInfo
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- CN111085270A CN111085270A CN201811238250.3A CN201811238250A CN111085270A CN 111085270 A CN111085270 A CN 111085270A CN 201811238250 A CN201811238250 A CN 201811238250A CN 111085270 A CN111085270 A CN 111085270A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
The invention discloses a preparation method of an ammonium octamolybdate-based supramolecular material catalyst, which comprises the following steps: sequentially reacting (NH)4)6Mo7O24·4H2O, bbi and water are added into a beaker, the mixture is continuously stirred for 1.5 to 2.5 hours at the temperature of between 25 and 35 ℃, the pH value of the system is adjusted to be 4.4 to 4.6 by using dilute hydrochloric acid with the concentration of 1mol/L, the mixture is transferred into a stainless steel reaction kettle with a Teflon liner, the temperature is kept constant at the temperature of 155 and 165 ℃ for 124 and 126 hours, and then the temperature is gradually reduced to the room temperature at the speed of 5 ℃/h, thus obtaining the catalyst. The method is simple, convenient, fast and easy to operate, and the prepared ammonium octamolybdate-based supramolecular material catalyst has high catalytic activity and excellent recyclable stability and can be prepared on a large scale.
Description
Technical Field
The invention relates to a preparation method of an ammonium octamolybdate-based supramolecular material catalyst.
Background
Epoxides are key raw materials of importance for the production of various chemical species, such as glycols, glycol ethers, alcohol amines, and polymers. Various compounds, including inorganic metal oxides and organometallic compounds, have been used so far for olefin epoxidation catalysts, generally using oxygen, ozone, hydrogen peroxide, organic peroxides as the oxidizing agent. In particular, catalytic oxidation processes using hydrogen peroxide as an oxidizing agent are attracting attention because hydrogen peroxide is a cheap, mild, environmentally friendly reagent that produces only water as a byproduct. Today, H2O2Has been successfully applied to propylene epoxidation reaction by taking TS-1 type molecular sieve as a catalyst in industry. However, in the case of homogeneous catalysis, although some molecular organometallic compounds such as CH3ReO3（MTO）、MoO2X2L2、CpMoO2Cl and the like have proven to be excellent catalysts for epoxidation reactions on a laboratory scale, but are expensive to produce due to these types of organometallic catalystsAnd the recycling of the process on an industrial scale, have not been applied to larger scale industrial processes to date. Polyoxometallate (POM)S) The interest of researchers is aroused due to the characteristics of good catalytic performance, such as high activity, good selectivity, controllable oxidation reduction at an atomic or molecular level, acidic property and the like.
Polyoxometallates have been extensively studied and used as oxidation catalysts in oxidation reactions over the last decades. Anion { PO4［WO(O2)2］4}3-The quaternary ammonium salt cation is combined into inorganic-organic hybrid salt which can be used as an epoxidation phase transfer catalyst under mild conditions with hydrogen peroxide as a main oxidant for various olefins. In addition, some Keggin or Lindqvist type hybrid polyoxometalates have also been found, e.g. [ C ]nmim］PW12O40And [ Cnmim］W6O19And the like, and may also be used as a catalyst for oxidation and esterification reactions.
Disclosure of Invention
The invention aims to provide a preparation method of an ammonium octamolybdate-based supramolecular material catalyst.
The invention is realized by the following technical scheme:
a preparation method of ammonium octamolybdate-based supramolecular material catalyst comprises the following steps: sequentially adding 10-20 parts of (NH)4)6Mo7O24•4H2Adding O, 7-13 parts of bbi and 55-65 parts of water into a beaker, continuously stirring the mixture for 1.5-2.5h at 25-35 ℃, adjusting the pH value of the system to 4.4-4.6 by using dilute hydrochloric acid with the concentration of 1mol/L, transferring the mixture into a stainless steel reaction kettle with a Teflon liner, keeping the temperature at 155-165 ℃ for 124-126h, and then reducing the temperature to room temperature at the rate of 5 ℃/h in a gradient manner to obtain the catalyst; the raw materials are in parts by weight.
Preferably, in the preparation method, the mixture is continuously stirred for 2 hours at 30 ℃.
Preferably, in the preparation method, the pH value of the system is adjusted to 4.5 by using dilute hydrochloric acid with the concentration of 1 mol/L.
Preferably, in the preparation method, the constant temperature is kept at 160 ℃ for 125 h.
The invention has the technical effects that:
the method is simple, convenient, fast and easy to operate, and the prepared ammonium octamolybdate-based supramolecular material catalyst has high catalytic activity and excellent recyclable stability and can be prepared on a large scale.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
A preparation method of ammonium octamolybdate-based supramolecular material catalyst comprises the following steps: sequentially adding 15 parts of (NH)4)6Mo7O24•4H2Adding O, 10 parts of bbi and 60 parts of water into a beaker, continuously stirring the mixture at 30 ℃ for 2h, adjusting the pH value of the system to 4.5 by using 1mol/L dilute hydrochloric acid, transferring the mixture into a stainless steel reaction kettle with a Teflon liner, keeping the temperature at 160 ℃ for 125h, and then, carrying out gradient cooling at the rate of 5 ℃/h to room temperature to obtain the product; the raw materials are in parts by weight.
Example 2
A preparation method of ammonium octamolybdate-based supramolecular material catalyst comprises the following steps: sequentially adding 10 parts of (NH)4)6Mo7O24•4H2Adding O, 7 parts of bbi and 55 parts of water into a beaker, continuously stirring the mixture for 1.5h at 25 ℃, adjusting the pH value of the system to 4.4 by using dilute hydrochloric acid with the concentration of 1mol/L, transferring the mixture into a stainless steel reaction kettle with a Teflon liner, keeping the temperature at 155 ℃ for 124h, and then, carrying out gradient cooling to room temperature at the speed of 5 ℃/h to obtain the product; the raw materials are in parts by weight.
Example 3
A preparation method of ammonium octamolybdate-based supramolecular material catalyst comprises the following steps: sequentially adding 20 parts of (NH)4)6Mo7O24•4H2O, 13 parts bbi and 65 parts water were added to a beaker, the mixture was stirred continuously at 35 ℃ for 2.5h, the pH of the system was adjusted to 4.6 with dilute hydrochloric acid having a concentration of 1mol/L, and the mixture was mixedTransferring the mixture into a stainless steel reaction kettle with a Teflon liner, keeping the temperature at 165 ℃ for 126h, and then cooling to room temperature at a rate of 5 ℃/h in a gradient manner to obtain the teflon-containing composite material; the raw materials are in parts by weight.
The method is simple, convenient, fast and easy to operate, and the prepared ammonium octamolybdate-based supramolecular material catalyst has high catalytic activity and excellent recyclable stability and can be prepared on a large scale.
Claims (4)
1. The preparation method of the ammonium octamolybdate-based supramolecular material catalyst is characterized by comprising the following steps of: sequentially adding 10-20 parts of (NH)4)6Mo7O24·4H2Adding O, 7-13 parts of bbi and 55-65 parts of water into a beaker, continuously stirring the mixture for 1.5-2.5h at 25-35 ℃, adjusting the pH value of the system to 4.4-4.6 by using dilute hydrochloric acid with the concentration of 1mol/L, transferring the mixture into a stainless steel reaction kettle with a Teflon liner, keeping the temperature at 155-165 ℃ for 124-126h, and then reducing the temperature to room temperature at the rate of 5 ℃/h in a gradient manner to obtain the catalyst; the raw materials are in parts by weight.
2. The method of claim 1, wherein: the mixture was stirred continuously at 30 ℃ for 2 h.
3. The method of claim 1, wherein: the pH value of the system is adjusted to 4.5 by using dilute hydrochloric acid with the concentration of 1 mol/L.
4. The method of claim 1, wherein: the temperature is kept constant at 160 ℃ for 125 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811238250.3A CN111085270A (en) | 2018-10-23 | 2018-10-23 | Preparation method of ammonium octamolybdate-based supramolecular material catalyst |
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| CN201811238250.3A CN111085270A (en) | 2018-10-23 | 2018-10-23 | Preparation method of ammonium octamolybdate-based supramolecular material catalyst |
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