CN107694597A - A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid - Google Patents

A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid Download PDF

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Publication number
CN107694597A
CN107694597A CN201711066001.6A CN201711066001A CN107694597A CN 107694597 A CN107694597 A CN 107694597A CN 201711066001 A CN201711066001 A CN 201711066001A CN 107694597 A CN107694597 A CN 107694597A
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CN
China
Prior art keywords
catalyst
trifluoromethylcinnaacid
acid
diatomite
synthesize
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Withdrawn
Application number
CN201711066001.6A
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Chinese (zh)
Inventor
罗志勤
林静霞
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Zhaoqing Hi Tech Zone National Science And Technology Co Ltd
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Zhaoqing Hi Tech Zone National Science And Technology Co Ltd
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Priority to CN201711066001.6A priority Critical patent/CN107694597A/en
Publication of CN107694597A publication Critical patent/CN107694597A/en
Withdrawn legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
    • B01J37/03Precipitation; Co-precipitation
    • B01J37/031Precipitation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/082Decomposition and pyrolysis
    • B01J37/088Decomposition of a metal salt
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/347Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
    • C07C51/353Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by isomerisation; by change of size of the carbon skeleton
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/584Recycling of catalysts

Abstract

A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid, its preparation method is, after potassium nitrate, potassium carbonate are added to the water into dissolving, adds diatomite, after stirring ageing a period of time, filtration drying, gained solid obtains catalyst after roasting.The catalyst can reduce sewage discharge for synthesizing m-TrifluoromethylcinnaAcid Acid, while reduce corrosion of the course of reaction to equipment.Moreover, diatomite is capable of the water of adsorption reaction generation, reaction is set to be more prone to carry out complete, raising product yield.Meanwhile catalyst can reuse after roasting, the production cost of reduction.

Description

A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid
Technical field
The present invention relates to a kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid.
Background technology
M-TrifluoromethylcinnaAcid Acid is a kind of polymer monomer and fine-chemical intermediate having many uses.In it is not only The side chain dressing agent of acid amides antibiotic, or the raw material of synthesis m-trifluoromethyl styrene, and m-trifluoromethyl styrene is poly- Compound can be used for making liquid crystal material;With some transistion metal compounds manufacture olefinic polymerization catalyst, obtain crystallization and The preferable polyolefin of the transparency;It can be used for the painting of thermoplastic resin film with polysiloxane grafted poly- m-trifluoromethyl styrene Layer, makes it have preferable flatness, the expelling water displacement of reservoir oil and anti-adhesion performance;In addition, it may also be used for manufacture mould inhibitor, electron surface The fine chemicals such as inorganic agent.
The synthetic method for the m-TrifluoromethylcinnaAcid Acid reported at present is mainly the Perkin contractings of m-Trifluoromethylbenzaldehyde Close, for yield 65% or so, yield is relatively low.
The content of the invention
The synthesis used catalyst of m-TrifluoromethylcinnaAcid Acid is generally potassium carbonate, sodium acetate, potassium acetate, triethylamine etc.. The reaction due to making catalyst with solid base, in building-up process can produce m-TrifluoromethylcinnaAcid Acid salt, it is necessary to in acid and, PH is adjusted just to obtain m-TrifluoromethylcinnaAcid Acid after acidity.And yield reduction is easily caused in the process, increase production Cost.A large amount of waste water are produced simultaneously, environment is impacted.
It is used to synthesize the catalyst of m-TrifluoromethylcinnaAcid Acid it is an object of the invention to provide a kind of, during the course of the reaction not With acid for adjusting pH value is added, m-TrifluoromethylcinnaAcid Acid is separated out, while reduce sewage discharge, improve product yield.
The present invention relates to a kind of diatomite catalyst for phenol hydroxylation.
In order to solve problem above, the present invention adopts the following technical scheme that realization:
A kind of catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid, its preparation method are to add potassium nitrate, potassium carbonate After being dissolved in water, diatomite is added, after stirring ageing a period of time, filtration drying, gained solid is catalyzed after roasting Agent.
Wherein, potassium nitrate used, potassium carbonate mass ratio are 1:1-2, potassium nitrate, carbonic acid potassium application rate and diatomite dosage matter Amount is than being 1:2-5.Digestion time is 8-18 hours, and sintering temperature is 300-500 DEG C.
The catalyst can reduce sewage discharge for synthesizing m-TrifluoromethylcinnaAcid Acid, while reduce course of reaction pair and set Standby corrosion.Moreover, diatomite is capable of the water of adsorption reaction generation, reaction is set to be more prone to carry out complete, raising product yield. Meanwhile catalyst can reuse after roasting, the production cost of reduction.
Specific embodiment
The present invention is described in detail below by specific embodiment.
Embodiment 1
Potassium nitrate 30g, potassium carbonate 50g are added in 200g water after dissolving, add 200g diatomite, stirred old 10 hours Afterwards, filtration drying, gained solid obtain catalyst after 350 DEG C of roastings.
This catalyst is used to synthesize m-TrifluoromethylcinnaAcid Acid, gained m-TrifluoromethylcinnaAcid Acid yield is 80%.
Embodiment 2
Potassium nitrate 50g, potassium carbonate 70g are added in 300g water after dissolving, add 250g diatomite, stirring ageing 8 hours Afterwards, filtration drying, gained solid obtain catalyst after 400 DEG C of roastings.
This catalyst is used to synthesize m-TrifluoromethylcinnaAcid Acid, gained m-TrifluoromethylcinnaAcid Acid yield is 76%.
Embodiment 3
25g potassium nitrate, 35g potassium carbonate are added in 250g water after dissolving, add 100g diatomite, stirring ageing 12 hours Afterwards, filtration drying, gained solid obtain catalyst after 350 DEG C of roastings.
This catalyst is used to synthesize m-TrifluoromethylcinnaAcid Acid, gained m-TrifluoromethylcinnaAcid Acid yield is 83%.
Embodiment 4
After the gained catalyst use of embodiment 3, after drying, it is re-used for synthesizing after being calcined 10 hours at 380 DEG C M-TrifluoromethylcinnaAcid Acid, gained m-TrifluoromethylcinnaAcid Acid yield are 72%.

Claims (3)

1. a kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid, its preparation method is, by potassium nitrate, potassium carbonate After being added to the water dissolving, diatomite is added, after stirring ageing a period of time, filtration drying, gained solid obtains after roasting Catalyst.
A kind of 2. catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid according to claims 1, it is characterised in that Potassium nitrate used, potassium carbonate mass ratio are 1:1-2, potassium nitrate, carbonic acid potassium application rate and diatomite dosage mass ratio are 1:2- 5。
A kind of 3. catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid according to claims 1, it is characterised in that Digestion time is 8-18 hours, and sintering temperature is 300-500 DEG C.
CN201711066001.6A 2017-11-02 2017-11-02 A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid Withdrawn CN107694597A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711066001.6A CN107694597A (en) 2017-11-02 2017-11-02 A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711066001.6A CN107694597A (en) 2017-11-02 2017-11-02 A kind of diatomite catalyst for being used to synthesize m-TrifluoromethylcinnaAcid Acid

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6001152A (en) * 1997-05-29 1999-12-14 Sinha; Rabindra K. Flue gas conditioning for the removal of particulates, hazardous substances, NOx, and SOx
CN101249450A (en) * 2008-03-28 2008-08-27 华东师范大学 Solid body base catalyst and applications for biological diesel oil synthesizing
US8809564B2 (en) * 2010-01-15 2014-08-19 National Cheng Kung University Platinum complex, manufacturing method thereof and platinum catalyst constructed thereby

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6001152A (en) * 1997-05-29 1999-12-14 Sinha; Rabindra K. Flue gas conditioning for the removal of particulates, hazardous substances, NOx, and SOx
CN101249450A (en) * 2008-03-28 2008-08-27 华东师范大学 Solid body base catalyst and applications for biological diesel oil synthesizing
US8809564B2 (en) * 2010-01-15 2014-08-19 National Cheng Kung University Platinum complex, manufacturing method thereof and platinum catalyst constructed thereby

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈平等: ""K2O/ Al2O3固体碱催化合成肉桂酸"", 《化学与生物工程》 *

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Application publication date: 20180216