CN107652174A - A kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid - Google Patents
A kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid Download PDFInfo
- Publication number
- CN107652174A CN107652174A CN201710768543.1A CN201710768543A CN107652174A CN 107652174 A CN107652174 A CN 107652174A CN 201710768543 A CN201710768543 A CN 201710768543A CN 107652174 A CN107652174 A CN 107652174A
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- CN
- China
- Prior art keywords
- iron
- molecular sieve
- sieve catalyst
- azelaic acid
- containing meso
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid, comprise the following steps：After unrighted acid, iron-containing meso molecular sieve catalyst, hexadecyltrimethylammonium chloride are mixed, 100 120 DEG C are heated with stirring to, after adding hydrogen chloride solution reaction, agitated kettle stirred crystallization separates out white powder, obtains azelaic acid solid after drying.It is an advantage of the invention that：It is easily isolated with reactant, is easy to reclaim, recycles, is discharged in reaction without a large amount of organic solvents, solid waste and toxic gas, beneficial to environment.
Description
Technical field
The invention belongs to technical field of chemical synthesis, and in particular to one kind is using unrighted acid with iron-containing meso molecule
Sieve as the method for catalyst preparation azelaic acid.
Background technology
Azelaic acid may be used as spices, lubricating oil, finish raw material and be used for alkyd resin, paint and chemical industry synthesis, big portion
Azelaic acid is divided to be used to produce dioctyl azelate (DOZ) plasticizer.The cold resistance that DOZ is used as cable, film, artificial leather etc. increases
Plasticity, volatility is small, resistance to ag(e)ing.It is synthetic method main at present to prepare azelaic acid using unrighted acids such as oleic acid,
But shortcoming is that the catalytic effect of solid catalyst is general, it is not easy and reactants separate.
The content of the invention
Therefore, it is an object of the invention to provide a kind of method that azelaic acid is prepared using unrighted acid, this method
Using iron-containing meso molecular sieve as catalyst, catalytic effect is notable, is easy to and reactants separate.Solution to problem is as follows：
1st, by unrighted acid, iron-containing meso molecular sieve catalyst and hexadecyltrimethylammonium chloride using mass ratio as
60：8：2 are mixed, and are heated with stirring to 100-120 DEG C, using mass ratio as：1：25 add hydrogen chloride solution reacts with mixed liquor,
React mixed liquor after terminating as being stirred in stirred tank, mixing time 6-8H, agitated kettle stirred crystallization separates out white
Color powder, dried in drying kettle, drying time 3-4H, drying temperature is 100-120 DEG C, obtains azelaic acid solid.
2nd, the mass ratio of above-mentioned unrighted acid, iron-containing meso molecular sieve catalyst and hexadecyltrimethylammonium chloride
For 60：8：2.
3rd, the mass ratio of above-mentioned hydrogen chloride and mixed liquor is：1：25.
4th, above-mentioned unrighted acid is oleic acid, leukotrienes and arachidonic acid.
5th, above-mentioned mixing time is 6-8H, and drying temperature is 100-120 DEG C, drying time 3-4H.
The inventive method is the catalyst significant effect using iron-containing meso molecular sieve as catalyst, easy with reactant
In separation, it is easy to reclaim, recycles, discharges, be beneficial to without a large amount of organic solvents, solid waste and toxic gas in reaction
Environment.
Embodiment
The present invention provides a kind of method that azelaic acid is prepared using unrighted acid, and this method is with iron-containing meso molecular sieve
For catalyst, catalytic effect is notable, is easy to and reactants separate.The unrighted acid, iron-containing meso molecular sieve catalyst
Mass ratio with hexadecyltrimethylammonium chloride is 60：8：2.The mass ratio of the hydrogen chloride and mixed liquor is：1：25.It is described
Unrighted acid is oleic acid, leukotrienes and arachidonic acid.The mixing time is 6-8H, and drying temperature is 100-120 DEG C,
Drying time is 3-4H.
Embodiment 1
Equipped with magnetic stirrer, thermometer, condenser pipe 500ml four-hole boiling flask in, add 50 grams of oleic acid, 8 grams contain
Iron mesopore molecular sieve, 2 grams of hexadecyltrimethylammonium chlorides, mass ratio is made into as 60：8：2 mixed liquor is heated with stirring to 100
DEG C, be added portionwise 200ml mass concentrations not 35% hydrogen chloride solution, be made into mass ratio with mixed liquor as 1：After 25 solution,
By mixed liquor as being stirred in stirred tank, mixing time is 6H until precipitation white powder, is doing in as drying kettle
4H is not dried under the conditions of 100 DEG C in dry temperature, obtains azelaic acid solid.
Claims (5)
1. a kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid, this method comprise the following steps：By unsaturated lipid
After fat acid, the mixing of iron-containing meso molecular sieve catalyst, hexadecyltrimethylammonium chloride, 100-120 DEG C is heated with stirring to, is added
After hydrogen chloride solution reaction, agitated kettle stirred crystallization separates out white powder, obtains azelaic acid solid after drying.
2. the method that a kind of iron-containing meso molecular sieve catalyst according to claim 1 prepares azelaic acid, it is characterized in that：Institute
The mass ratio for stating unrighted acid, iron-containing meso molecular sieve catalyst and hexadecyltrimethylammonium chloride is 60：8：2.
3. the method that a kind of iron-containing meso molecular sieve catalyst according to claim 1 prepares azelaic acid, it is characterized in that：Institute
The mass ratio for stating hydrogen chloride and mixed liquor is：1：25.
4. the method that a kind of iron-containing meso molecular sieve catalyst according to claim 1 prepares azelaic acid, it is characterized in that：Institute
It is oleic acid, leukotrienes and arachidonic acid to state unrighted acid.
5. the method that a kind of iron-containing meso molecular sieve catalyst according to claim 1 prepares azelaic acid, it is characterized in that：Institute
It is 6-8H to state mixing time, and drying temperature is 100-120 DEG C, drying time 3-4H.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710768543.1A CN107652174A (en) | 2017-08-31 | 2017-08-31 | A kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710768543.1A CN107652174A (en) | 2017-08-31 | 2017-08-31 | A kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107652174A true CN107652174A (en) | 2018-02-02 |
Family
ID=61129000
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710768543.1A Pending CN107652174A (en) | 2017-08-31 | 2017-08-31 | A kind of method that iron-containing meso molecular sieve catalyst prepares azelaic acid |
Country Status (1)
| Country | Link |
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| CN (1) | CN107652174A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198948A (en) * | 2010-03-26 | 2011-09-28 | 北京化工大学 | Method for preparing mesoporous molecular sieve Fe-MCM-41 with high iron content |
| CN103467273A (en) * | 2013-09-24 | 2013-12-25 | 辽宁石油化工大学 | Method for preparing azelaic acid from rare earth Ce-loaded mesoporous molecular sieve catalyst |
| CN104447279A (en) * | 2014-12-05 | 2015-03-25 | 辽宁石油化工大学 | Method for synthesizing anchoic acid through combined oxidation of hydrogen peroxide and potassium permanganate |
| CN104925827A (en) * | 2015-05-22 | 2015-09-23 | 北京化工大学 | Transition-metal-including crystal-structure mesoporous molecular sieve Cry-Fe and preparation method thereof |
-
2017
- 2017-08-31 CN CN201710768543.1A patent/CN107652174A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198948A (en) * | 2010-03-26 | 2011-09-28 | 北京化工大学 | Method for preparing mesoporous molecular sieve Fe-MCM-41 with high iron content |
| CN103467273A (en) * | 2013-09-24 | 2013-12-25 | 辽宁石油化工大学 | Method for preparing azelaic acid from rare earth Ce-loaded mesoporous molecular sieve catalyst |
| CN104447279A (en) * | 2014-12-05 | 2015-03-25 | 辽宁石油化工大学 | Method for synthesizing anchoic acid through combined oxidation of hydrogen peroxide and potassium permanganate |
| CN104925827A (en) * | 2015-05-22 | 2015-09-23 | 北京化工大学 | Transition-metal-including crystal-structure mesoporous molecular sieve Cry-Fe and preparation method thereof |
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Application publication date: 20180202 |
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