CN107694557A - A kind of macro porous silica gel loaded catalyst for acylation reaction - Google Patents
A kind of macro porous silica gel loaded catalyst for acylation reaction Download PDFInfo
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- CN107694557A CN107694557A CN201710991394.5A CN201710991394A CN107694557A CN 107694557 A CN107694557 A CN 107694557A CN 201710991394 A CN201710991394 A CN 201710991394A CN 107694557 A CN107694557 A CN 107694557A
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- silica gel
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
A kind of macro porous silica gel loaded catalyst for acylation reaction, by（a）Zinc chloride,（b）Two kinds in copper chloride, aluminium chloride, lanthanum nitrate, zirconium nitrate or the mixture more than two kinds,（c）Macro porous silica gel forms.Macro porous silica gel catalyst has acid and porous, and it has, and selectivity is good, active high, service life length, recyclable regeneration, it is free from environmental pollution many advantages, such as, be highly suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of macro porous silica gel loaded catalyst for acylation reaction.
Background technology
Acylation reaction is an important major class methodology of organic synthesis, and many cosmetics, aromatic, medicine, agricultural
Industrial processes involved by the chemical products such as chemicals or in-between product.At present, this reaction is most of in industry uses
Catalyst be homogeneous catalyst, including acid (AlCl3、BF3、ZnCl2、TiCl4、FeCl3Deng) and acid (HF, H2SO4、HCl、
H3PO4, p-methyl benzenesulfonic acid etc.).Although homogeneous catalyst technology relative maturity, exist in industry using homogeneous catalyst is most
Etching apparatus；Catalyst itself has corrosivity, operates abnormally dangerous；Need neutralization reactant and processing substantial amounts of soluble
Salt, and these operations can all reduce the conversion ratio, yield and selectivity of reaction, deficiency in economic performance.Therefore, from economy and environment
Angle considers to be badly in need of developing a kind of novel solid acid catalyst.
People have given this respect research to the pay attention to day by day of environmental problem with great power.The use of solid acid catalyst
It is the important channel for realizing homogeneous reaction heterogeneouss, reaction terminates rear catalyst and product is easily separated, solves returning for catalyst
The problems such as receiving, be repeated several times or recycling.The advantages that no waste discharge and simple technological process, in development of resources, save energy
Source and environmental protection etc. have great importance.
The content of the invention
The present invention relates to a kind of macro porous silica gel loaded catalyst for acylation reaction.
In order to solve problem above, the present invention adopts the following technical scheme that realization：
A kind of macro porous silica gel loaded catalyst for acylation reaction, it is characterised in that by (a) zinc chloride, (b) chlorine
Change two kinds in copper, aluminium chloride, lanthanum nitrate, zirconium nitrate or the mixture more than two kinds, (c) macro porous silica gel composition.
Method for preparing catalyst is：By two kinds in (a) zinc chloride, (b) copper chloride, aluminium chloride, lanthanum nitrate, zirconium nitrate or
The components such as mixture, (c) macro porous silica gel more than two kinds are added to the water stir and be aged after, dry and after grinding, through roasting
Catalyst is produced after burning.
(a) mass ratio of (b) (c) component is (a)：(b)：(c)=1：1~1.5：3~8.
Macro porous silica gel is a kind of silica gel of special type, a kind of high activity sorbing material as other silica gel, belongs to amorphous
State material, its chemical molecular formula are mSiO2·nH2O.Not soluble in water and any solvent, nonpoisonous and tasteless, chemical property is stable, except strong
Do not reacted outside alkali, hydrofluoric acid with any material.The silica gel of various models because its manufacture method is different formed it is different micro-
Pore structure.It is that pore volume is big that it, which is distinguished with the maximum feature of other silica gel, that is, adsorbance is very big, and bulk specific weight is very light.At present
The macro porous silica gel of domestic production, its pore volume are up to 1.7ml/g.
Metallic compound is still the most frequently used a kind of acidic catalyst, is fixed on carrier and is prepared into support type and urges
Agent, reaction terminate rear catalyst and easily removed, and solve the recovery of catalyst.Meanwhile macro porous silica gel catalyst has acidity
And porous, it has, and selectivity is good, active high, service life length, recyclable regeneration, it is free from environmental pollution many advantages, such as, it is non-
Often it is applied to industrialized production.
Specific embodiment
The present invention is described in detail below by specific embodiment.
Embodiment 1
The components such as zinc chloride 100g, copper chloride 50g, aluminium chloride 30g, lanthanum nitrate 25g, macro porous silica gel 350g are added
Stir in 1000g water, and after being aged 10 hours, dry and after being ground into 50 mesh, produce after 4 hours and urge through 400 DEG C of roastings
Agent.
This catalyst is used for the acylation reaction of 1- methoxynaphthalenes and acetic acid, yield 95%.
Embodiment 2
The components such as 50g zinc chloride, 30g aluminium chloride, 15g lanthanum nitrates, 30g zirconium nitrate 400g macro porous silica gels are added into 1500g
Stir in water, and after being aged 12 hours, dry and after being ground into 80 mesh powder, catalysis is produced after 8 hours through 350 DEG C of roastings
Agent.
This catalyst is used for methyl phenyl ethers anisole and acetic anhydride, the yield of acetanisole is 94%.
Embodiment 3
By groups such as 100g zinc chloride, 55g copper chlorides, 35g aluminium chloride, 15g lanthanum nitrates, 40g zirconium nitrate 500g macro porous silica gels
Point add in 2000g water and to stir, and after being aged 18 hours, dry and after being ground into 100 mesh, be calcined 12 hours through 350 DEG C
After produce catalyst.
This catalyst is used for methyl phenyl ethers anisole and excess acetyl chloride, the yield of methoxyacetophenone is 85%, ortho para position body ratio
Example is 90：10.
Claims (3)
- A kind of 1. macro porous silica gel loaded catalyst for acylation reaction, it is characterised in that by（a）Zinc chloride,（b）Chlorination Two kinds in copper, aluminium chloride, lanthanum nitrate, zirconium nitrate or the mixture more than two kinds,（c）Macro porous silica gel forms.
- 2. according to the catalyst described in claims 1, other method for preparing catalyst for being characterised by described are：Will（a） Zinc chloride,（b）Two kinds in copper chloride, aluminium chloride, lanthanum nitrate, zirconium nitrate or the mixture more than two kinds,（c）Macro porous silica gel etc. Component is added to the water stir and be aged after, dry and after grinding, catalyst produced after fired.
- 3. according to the catalyst described in claims 1, it is characterised in that（a）（b）（c）The mass ratio of component is（a）:（b）: （c）=1:1~1.5:3~8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710991394.5A CN107694557A (en) | 2017-10-23 | 2017-10-23 | A kind of macro porous silica gel loaded catalyst for acylation reaction |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710991394.5A CN107694557A (en) | 2017-10-23 | 2017-10-23 | A kind of macro porous silica gel loaded catalyst for acylation reaction |
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| CN107694557A true CN107694557A (en) | 2018-02-16 |
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| CN201710991394.5A Pending CN107694557A (en) | 2017-10-23 | 2017-10-23 | A kind of macro porous silica gel loaded catalyst for acylation reaction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662166A (en) * | 2020-05-28 | 2020-09-15 | 吴赣药业（苏州）有限公司 | Preparation method of 5-bromo-2-chloro-4' -ethoxy diphenylmethane |
| CN111905778A (en) * | 2020-08-24 | 2020-11-10 | 浙江工业大学台州研究院 | Supported catalyst, preparation method thereof and application thereof in synthesis of ethylbenzyl chloride |
Citations (5)
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| JP2002095971A (en) * | 2000-09-22 | 2002-04-02 | Chemiprokasei Kaisha Ltd | Friedel-crafts catalyst and method for producing alkylated aromatic compound or benzoylated aromatic compound by using the same |
| CN1613559A (en) * | 2004-09-28 | 2005-05-11 | 北京化工大学 | Preparation for hydrophobic solid acid catalyst |
| WO2007044270A1 (en) * | 2005-10-06 | 2007-04-19 | Albemarle Corporation | Process for producing high purity ketones by friedel-crafts acylation at low temperature |
| CN101733142A (en) * | 2009-12-16 | 2010-06-16 | 南京德美世创化工有限公司 | Supported solid acid catalyst, preparation method thereof and use thereof |
| CN102302948A (en) * | 2011-06-21 | 2012-01-04 | 西北师范大学 | Benzenesulfonic acid catalyst supported on silica gel, as well as preparation and application thereof |
-
2017
- 2017-10-23 CN CN201710991394.5A patent/CN107694557A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002095971A (en) * | 2000-09-22 | 2002-04-02 | Chemiprokasei Kaisha Ltd | Friedel-crafts catalyst and method for producing alkylated aromatic compound or benzoylated aromatic compound by using the same |
| CN1613559A (en) * | 2004-09-28 | 2005-05-11 | 北京化工大学 | Preparation for hydrophobic solid acid catalyst |
| WO2007044270A1 (en) * | 2005-10-06 | 2007-04-19 | Albemarle Corporation | Process for producing high purity ketones by friedel-crafts acylation at low temperature |
| CN101733142A (en) * | 2009-12-16 | 2010-06-16 | 南京德美世创化工有限公司 | Supported solid acid catalyst, preparation method thereof and use thereof |
| CN102302948A (en) * | 2011-06-21 | 2012-01-04 | 西北师范大学 | Benzenesulfonic acid catalyst supported on silica gel, as well as preparation and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 秦浩正: "《中学生学习辞典：化学卷》", 30 September 2012 * |
| 钟邦克: "《固体酸催化的酯化和酰化》", 30 April 2007 * |
| 钟邦克: "《精细化工过程催化作用》", 31 August 2002 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662166A (en) * | 2020-05-28 | 2020-09-15 | 吴赣药业（苏州）有限公司 | Preparation method of 5-bromo-2-chloro-4' -ethoxy diphenylmethane |
| CN111905778A (en) * | 2020-08-24 | 2020-11-10 | 浙江工业大学台州研究院 | Supported catalyst, preparation method thereof and application thereof in synthesis of ethylbenzyl chloride |
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Application publication date: 20180216 |