CN109320416A - Application of Anhydrous Calcium Sulfate in Synthesis of Methyl Stearate - Google Patents
Application of Anhydrous Calcium Sulfate in Synthesis of Methyl Stearate Download PDFInfo
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- CN109320416A CN109320416A CN201811338451.0A CN201811338451A CN109320416A CN 109320416 A CN109320416 A CN 109320416A CN 201811338451 A CN201811338451 A CN 201811338451A CN 109320416 A CN109320416 A CN 109320416A
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- reaction
- esterification
- application
- catalyst
- stearic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention discloses a kind of application of dead plaster in synthesis methyl stearate；Catalyst amount of the invention is ‰ ~ 5wt of 1wt ‰ of the ester synthesis reaction stearic acid starting material；Esterification is carried out in polytetrafluoroethylene (PTFE) water heating kettle, and esterification reaction temperature is 100 DEG C ~ 180 DEG C, and the reaction time is 3 ~ 12h.In the present invention, catalyst and reaction product convenient separation, are separated by filtration catalyst after reaction, reusable after drying.Catalyst of the present invention is a kind of cheap dead plaster, environment friendly and pollution-free and can be recycled.
Description
Technical field
The invention belongs to catalytic synthetic techniques fields, specifically, are related to a kind of dead plaster in synthesis stearic acid first
Application in ester.
Background technique
Esters are that made of being gone as inorganic acid or organic acid and alcohol progress esterification contracting, have wide market to need
It asks, traditional esterification generally uses sulfuric acid as catalysts, although sulfuric acid catalysis activity is high, low in cost, in life
Meeting severe corrosion equipment, causes the side reactions such as organic carbon, oxidation, etherificate, sulfonation, other kinds of catalyst during producing
If heteropoly acid was difficult to carry out industrialized production because of the problems such as cost, look for a kind of novel that catalyst for esterification reaction is compeled
The eyebrows and eyelashes.
Dead plaster is the catalyst that a kind of catalytic activity is higher, cheap, and there is no the corrosion to equipment
Phenomenon, catalyst and convenient product separation after reaction, catalyst is reusable after drying, has and widely answers very much
Use prospect.
Summary of the invention
In order to overcome the shortcomings of existing catalyst, it is stearic in synthesis that the purpose of the present invention is to provide a kind of dead plasters
Application in sour methyl esters.Dead plaster of the invention as methyl stearate synthetic catalyst, it is low in cost, be easily isolated,
Reusable, catalytic activity is high.Technical solution of the present invention is specifically described as follows.
The present invention provides a kind of application of dead plaster in synthesis methyl stearate.
Preferably, application method is as follows: using stearic acid and methanol as raw material, using dead plaster as catalyst,
Esterification occurs in solvent heat kettle and synthesizes methyl stearate.
Preferably, catalyst amount is stearic ‰ ~ 5wt of 1wt ‰.
Preferably, the molar ratio of stearic acid and methanol is 1:2 ~ 1:5, and esterification reaction temperature is 120 DEG C ~ 180 DEG C, and esterification is anti-
It is 3 ~ 12h between seasonable.It is further preferred that esterification reaction temperature is 150 DEG C ~ 180 DEG C, reaction time of esterification is 4 ~ 12h；More into
One step is preferred, and esterification reaction temperature is 160 ~ 180 DEG C, and reaction time of esterification is 8 ~ 12h.
Compared with prior art, the invention has the following advantages that
Catalyst of the invention using dead plaster as synthesis methyl stearate, reaction is mild, the by-product generated in reaction
The shortcomings that less, esterification yield is high, and the color of product is good, overcomes traditional catalyst corrosion equipment, catalyst is easy after reaction
In separation and after simple process it is reusable.Dead plaster is cheap to be easy to get, and will not generate pollution to environment,
It is a kind of excellent environmentally friendly catalyst.The synthesis technology of methyl stearate is relatively easy in the present invention, investment and energy
Consume it is less, be convenient for industrial production.
Specific embodiment
Below with reference to embodiment, invention is further described in detail, but protection scope of the present invention be not limited to it is following
Embodiment.
Embodiment 1
30g stearic acid, 10.137g methanol and 0.03g dead plaster are added in the anti-water heating kettle of polytetrafluoroethylene (PTFE), stirs evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 120 DEG C afterwards, after reaction system is cooled to room temperature, uniform stirring reaction
Product in kettle, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 30.43%.Reaction kettle is placed in thermostat water bath and is heated to 80 DEG C, filters the substance in reaction kettle with funnel,
Staying on filter paper is calcium sulfate, obtains dead plaster after 250 DEG C of drying, is by simple filtration, separation and drying
The recycling of catalyst can be achieved.
Embodiment 2
30g stearic acid, 10.137g methanol and 0.03g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 150 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 60.99%.
Embodiment 3
30g stearic acid, 10.137g methanol and 0.09g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 150 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 61.45%.
Embodiment 4
30g stearic acid, 10.137g methanol and 0.15g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 150 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 62.70%.
Embodiment 5
30g stearic acid, 10.137g methanol and 0.03g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 180 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 78.05%.
Embodiment 6
30g stearic acid, 10.137g methanol and 0.09g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 180 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 79.15%.
Embodiment 7
30g stearic acid, 10.137g methanol and 0.15g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 180 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 79.33%.
Embodiment 8
30g stearic acid, 10.137g methanol and 0.09g dead plaster are added in polytetrafluoroethylene (PTFE) water heating kettle, after mixing evenly
Reaction kettle is placed in baking oven the solvent thermal reaction 4h at 160 DEG C, after reaction system is cooled to room temperature, uniform stirring reaction kettle
In product, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto be added 2 ~ 3 drop phenolphthalein solutions, use
0.05moL/L KOH solution is titrated to red, calculates stearic conversion ratio according to KOH dosage.Titration results show stearic acid
Conversion ratio be 68.20%.
Embodiment 9
Reaction kettle in embodiment 8 is placed in 120 DEG C of baking oven after placing 4h and is taken out, added thereto after reaction system is cooling
Enter 10.137g methanol, reaction kettle is placed in baking oven the solvent thermal reaction 4h at 160 DEG C after mixing evenly, it is cold to reaction system
But to after room temperature, product in uniform stirring reaction kettle, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto
2 ~ 3 drop phenolphthalein solutions are added, are titrated to red with 0.05moL/L KOH solution, stearic conversion is calculated according to KOH dosage
Rate.Titration results show that stearic conversion ratio is 86.72%.
Embodiment 10
Reaction kettle in embodiment 9 is placed in 120 DEG C of baking oven after placing 4h and is taken out, added thereto after reaction system is cooling
Enter 10.137g methanol, reaction kettle is placed in baking oven the solvent thermal reaction 4h at 160 DEG C after mixing evenly, it is cold to reaction system
But to after room temperature, product in uniform stirring reaction kettle, take 2g product be dissolved in 50mL, 95% ethanol solution in, thereto
2 ~ 3 drop phenolphthalein solutions are added, are titrated to red with 0.05moL/L KOH solution, stearic conversion is calculated according to KOH dosage
Rate.Titration results show that stearic conversion ratio is 96.34%.
Claims (6)
1. application of the dead plaster in synthesis methyl stearate.
2. application as described in claim 1, which is characterized in that application method is as follows: using stearic acid and methanol as raw material, with
Dead plaster occurs esterification in solvent heat kettle and synthesizes methyl stearate as catalyst.
3. application as claimed in claim 2, which is characterized in that catalyst amount is stearic ‰ ~ 5wt of 1wt ‰.
4. application as claimed in claim 2, which is characterized in that the molar ratio of stearic acid and methanol is 1:2 ~ 1:5, esterification
Temperature is 120 DEG C ~ 180 DEG C, and reaction time of esterification is 3 ~ 12h.
5. application as claimed in claim 2, which is characterized in that esterification reaction temperature is 150 DEG C ~ 180 DEG C, reaction time of esterification
For 4 ~ 12h.
6. application as claimed in claim 2, which is characterized in that esterification reaction temperature is 160 DEG C, reaction time of esterification is 8 ~
12h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811338451.0A CN109320416A (en) | 2018-11-12 | 2018-11-12 | Application of Anhydrous Calcium Sulfate in Synthesis of Methyl Stearate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811338451.0A CN109320416A (en) | 2018-11-12 | 2018-11-12 | Application of Anhydrous Calcium Sulfate in Synthesis of Methyl Stearate |
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| CN109320416A true CN109320416A (en) | 2019-02-12 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09188690A (en) * | 1996-01-08 | 1997-07-22 | Mitsubishi Chem Corp | Production of sucrose fatty acid ester |
| US20090126262A1 (en) * | 2007-11-20 | 2009-05-21 | Board Of Trustees Of Michigan State University | Process for producing mixed esters of fatty acids as biofuels |
| CN101703939A (en) * | 2009-03-10 | 2010-05-12 | 辽宁石油化工大学 | Application of calcium sulfate whisker as catalyst for ester synthesis |
| CN101703938A (en) * | 2009-03-06 | 2010-05-12 | 东北大学 | Application of calcium sulfate whisker as catalyst for ester exchange reaction |
| CN102351690A (en) * | 2011-09-08 | 2012-02-15 | 安徽佳先功能助剂股份有限公司 | Method for preparing methyl stearate |
-
2018
- 2018-11-12 CN CN201811338451.0A patent/CN109320416A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09188690A (en) * | 1996-01-08 | 1997-07-22 | Mitsubishi Chem Corp | Production of sucrose fatty acid ester |
| US20090126262A1 (en) * | 2007-11-20 | 2009-05-21 | Board Of Trustees Of Michigan State University | Process for producing mixed esters of fatty acids as biofuels |
| CN101703938A (en) * | 2009-03-06 | 2010-05-12 | 东北大学 | Application of calcium sulfate whisker as catalyst for ester exchange reaction |
| CN101703939A (en) * | 2009-03-10 | 2010-05-12 | 辽宁石油化工大学 | Application of calcium sulfate whisker as catalyst for ester synthesis |
| CN102351690A (en) * | 2011-09-08 | 2012-02-15 | 安徽佳先功能助剂股份有限公司 | Method for preparing methyl stearate |
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Application publication date: 20190212 |
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