CN102351692A - Preparation method for dimethyl sebacate - Google Patents
Preparation method for dimethyl sebacate Download PDFInfo
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- CN102351692A CN102351692A CN2011103046978A CN201110304697A CN102351692A CN 102351692 A CN102351692 A CN 102351692A CN 2011103046978 A CN2011103046978 A CN 2011103046978A CN 201110304697 A CN201110304697 A CN 201110304697A CN 102351692 A CN102351692 A CN 102351692A
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Abstract
The invention belongs to the field of chemical product preparation and particularly relates to a preparation method for dimethyl sebacate. A production method for the dimethyl sebacate comprises the following steps of esterification reaction and rectification process and has the concrete steps that: sebacic acid is mixed with methanol, then, solid catalysts are added, the esterification reaction is carried out, and then, products are purified through a rectification process. The method has the beneficial effect that the consumption mol ratio of the sebacic acid to the methanol is 1/0.9 to 1.2. Compared with the prior art, the method has the advantages that the consumption of the methanol is greatly saved, about 3 percent of the cost is saved, the solid acid is used as catalysts, the reaction efficiency is greatly improved, in addition, compared with the prior art adopting concentrated sulfuric acid as catalysts, the method has the advantage that the solid catalysts adopted by the method can be cyclically utilized, and compared with the method adopting liquid catalysts, the method has the advantage that about 5 percent of the cost is saved.
Description
Technical field
The invention belongs to the Chemicals preparation field, be specifically related to a kind of method of dimethyl sebacate preparation.
Background technology
The method that prepare at present dimethyl sebacate mainly is that sebacic acid and methyl alcohol are mixed with certain proportion, under the effect of catalyzer, treat that sebacic acid dissolves fully after, carry out esterification, treat that temperature reduces to after the solution formation separation surface, isolate water; And then add sebacic acid and carry out second with methyl alcohol and go on foot the esterification esterification, in above esterification, the general catalyzer that uses is the vitriol oil; With liquid as catalyzer; Can't reclaim, not only cost is higher, and operator also have certain danger when work.
CN1025916C discloses a kind of preparation method of dimethyl sebacate; This method be with sebacic acid, methyl alcohol is thick is raw material, is catalyzer with the vitriol oil, in the esterification dehydration of following minute three step of the condition of heating, dealcoholysis; Through washing, neutralization, washing, underpressure distillation, make dimethyl sebacate again.This method adopts three step esterifications, and its step is more numerous and diverse, and the amount ratio of methyl alcohol is bigger, and the amount ratio that sebacic acid and methyl alcohol are thick is 1:2-3, and in real reaction, the amount of methyl alcohol is excessive, so the cost of this method generation dimethyl sebacate is higher; In addition, its catalyzer that uses is the vitriol oil, and cost is higher, and the staff operates and also has certain danger.In addition, adopt the vitriol oil to make catalyzer, the product color that obtains is bad, while vitriol oil corrosive equipment, and produce a large amount of acid waste liquid contaminate environment.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides a kind of method of dimethyl sebacate preparation, this method adopts solid catalyst, compares with the liquid catalyst that adopts before, has not only shortened the reaction times, has also practiced thrift cost.
The present invention realizes through following technical scheme:
The preparation method of dimethyl sebacate of the present invention comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:0.9～1.2:0.004～0.008;
(2) get and account for that methyl alcohol total mass fractional 30～50% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds solid catalyst, and described solid catalyst is SiO
2-Al
2O
3, B
2O
3-Al
2O
3, at least a in the oligomerization of propene; The solid catalyst consumption that is added is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature and reach 70～85 ℃ of insulation 1h, carry out esterification first time, esterification time is 3～4h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110～125 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 75～85 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 65～75 ℃ of concentration 2.0～6.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09Mpa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096Mpa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closing thermal oil has the turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.
Preferably, the preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1.0:0.005;
(2) get and account for that methyl alcohol total mass fractional 40% joins in the esterifying kettle in the step (1), close to put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step (1) again, adds solid catalyst, and described solid catalyst is SiO
2-Al
2O
3The solid catalyst consumption that is added is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature and reach 75 ℃ of insulation 1h, carry out esterification first time, esterification time is 3h, for the first time after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step (1) is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 80 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 70 ℃ of concentration 4.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, opens the thermal oil valve and heats up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09Mpa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096Mpa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.
Beneficial effect of the present invention is:
(1) the present invention is a raw material with dimethyl sebacate and methyl alcohol; Adopt solid catalyst to quicken its reaction, the consumption mol ratio of sebacic acid and methyl alcohol is 1:0.9～1.2 among the present invention, with respect to prior art; Practiced thrift the consumption of methyl alcohol greatly, practiced thrift cost and be about 3%;
(2) adopt solid to make catalyzer and not only improved reaction efficiency greatly; And compare as catalyzer with the vitriol oil of available technology adopting; Its advantage is can recycle; Compare with liquid catalyst; It has reduced about 5% cost; And the solid catalyst that adopts of the present invention can etching apparatus, thereby has prolonged the work-ing life of equipment;
(3) among the present invention, the usage quantity of alkali will be lacked with respect to prior art, also reduces about 3% production cost.
Embodiment
Below in conjunction with specific embodiment the present invention is done explanation further,, but therefore do not limit the present invention so that those skilled in the art more understands the present invention.
Embodiment 1
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:0.9:0.004;
(2) get and account for that methyl alcohol total mass fractional 30% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds solid catalyst SiO
2-Al
2O
3Its add-on is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature time insulation 1h that reaches 70 ℃ of left and right sides, carry out esterification first time, esterification time is 3～4h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110～125 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 75 ℃, the pH value of using the sodium carbonate solution of 65 ℃ of concentration 2.0%, temperature to be neutralized to the reaction ester solution is 7.5;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09Mpa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096Mpa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.Products obtained therefrom is a colourless transparent liquid, is characterized by dimethyl sebacate through infrared spectra and proton nmr spectra.
| Do not add catalyzer | The vitriol oil is made catalyzer | Method of the present invention | |
| Reaction times/h | 20h | 10h | 3-4h |
| Productive rate/% | 84.3 | 92.3 | 97.5. |
Embodiment 2
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1:0.005;
(2) get and account for that methyl alcohol total mass fractional 30% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds solid catalyst B
2O
3-Al
2O
3Its add-on is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature time insulation 1h that reaches 80 ℃ of left and right sides, carry out esterification first time, esterification time is about 3h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 120 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 75 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 65 ℃ of concentration 2.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.Products obtained therefrom is a colourless transparent liquid, is characterized by dimethyl sebacate through infrared spectra and proton nmr spectra.
The productive rate of dimethyl sebacate is 97.3%.
Embodiment 3
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1.1:0.004;
(2) get and account for that methyl alcohol total mass fractional 40% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds solid catalyst SiO
2-Al
2O
3Its add-on is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature time insulation 1h that reaches 85 ℃ of left and right sides, carry out esterification first time, esterification time is 3～4h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 75 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 65 ℃ of concentration 2.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.Products obtained therefrom is a colourless transparent liquid, is characterized by dimethyl sebacate through infrared spectra and proton nmr spectra.
The productive rate of dimethyl sebacate is 97.2%.
Embodiment 4
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1.2:0.008;
(2) get and account for that methyl alcohol total mass fractional 50% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds solid catalyst SiO
2-Al
2O
3Its add-on is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature time insulation 1h that reaches 85 ℃ of left and right sides, carry out esterification first time, esterification time is 4h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 125 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 85 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 75 ℃ of concentration 6.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.Products obtained therefrom is a colourless transparent liquid, is characterized by dimethyl sebacate through infrared spectra and proton nmr spectra.
The productive rate of dimethyl sebacate is 97.0%.
Embodiment 5
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:0.9:0.004;
(2) get and account for that methyl alcohol total mass fractional 30% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds solid catalyst B
2O
3-Al
2O
3Its add-on is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature time insulation 1h that reaches 70 ℃ of left and right sides, carry out esterification first time, esterification time is 3h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 75 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 65 ℃ of concentration 2.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article, and products obtained therefrom is a colourless transparent liquid, is characterized by dimethyl sebacate through infrared spectra and proton nmr spectra.
The productive rate of dimethyl sebacate is 97.4%.
Embodiment 6
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1.1:0.006;
(2) get and account for that methyl alcohol total mass fractional 30% joins in the esterifying kettle in the step 1, close and put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step 1 again, adds the solid catalyst oligomerization of propene; Its add-on is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature time insulation 1h that reaches 70 ℃ of left and right sides, carry out esterification first time, esterification time is 3.5h, after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 120 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step 1 is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 80 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 65 ℃ of concentration 4.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, open the thermal oil valve and heat up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.Products obtained therefrom is a colourless transparent liquid, is characterized by dimethyl sebacate through infrared spectra and proton nmr spectra.
The productive rate of dimethyl sebacate is 97.3%.
Embodiment 7
The preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1.0:0.005;
(2) get and account for that methyl alcohol total mass fractional 40% joins in the esterifying kettle in the step (1), close to put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step (1) again, adds solid catalyst, and described solid catalyst is SiO
2-Al
2O
3The solid catalyst consumption that is added is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature and reach 75 ℃ of insulation 1h, carry out esterification first time, esterification time is 3h, for the first time after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step (1) is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 80 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 70 ℃ of concentration 4.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, opens the thermal oil valve and heats up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.
The productive rate of dimethyl sebacate is 97.7%.
Claims (2)
1. the preparation method of dimethyl sebacate comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:0.9～1.2:0.004～0.008;
(2) get and account for that methyl alcohol total mass fractional 30～50% joins in the esterifying kettle in the step (1), close to put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step (1) again, adds solid catalyst, and described solid catalyst is SiO
2-Al
2O
3, B
2O
3-Al
2O
3, at least a in the oligomerization of propene; The solid catalyst consumption that is added is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature and reach 70～85 ℃ of insulation 1h, carry out esterification first time, esterification time is 3～4h, for the first time after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110～125 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step (1) is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 75～85 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 65～75 ℃ of concentration 2.0～6.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, opens the thermal oil valve and heats up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.
2. the preparation method of dimethyl sebacate as claimed in claim 1 comprises following step:
Esterification
(1) prepares material by following mol ratio: sebacic acid: methyl alcohol: catalyzer=1:1.0:0.005;
(2) get and account for that methyl alcohol total mass fractional 40% joins in the esterifying kettle in the step (1), close to put the alcohol door, turn on agitator drops into whole sebacic acid of getting ready in the step (1) again, adds solid catalyst, and described solid catalyst is SiO
2-Al
2O
3The solid catalyst consumption that is added is 0.15% of a sebacic acid massfraction, fastens cover, drives registering instrument;
(3) open steam valve and be warming up to the liquid temperature and reach 75 ℃ of insulation 1h, carry out esterification first time, esterification time is 3h, for the first time after the esterification, continues to be warming up to 90 ℃ and begin to steam pure;
(4) when temperature rises to 110 ℃, begin to add continuously alcohol, the methyl alcohol of the surplus in the step (1) is all added esterifying kettle carry out the secondary esterification, add pure speed≤300L/h, the secondary esterification temperature is not more than 140 ℃;
Rectification process
(1) when liquid temperature drop to 80 ℃, is neutralized to the pH value 7.5 of reaction ester solution with the sodium carbonate solution of 70 ℃ of concentration 4.0%, temperature;
(2) ejector priming will bleed off in the thick ester suction rectifying still of waste lye, opens the thermal oil valve and heats up, and when the rectifying still temperature rose to more than 150 ℃, vacuum tightness was closed pump at 0.09MPa, opens slide valve pump;
(3) rise to more than 160 ℃ when the rectifying still temperature, vacuum tightness begins to reflux when 0.096MPa, and return time at least one hour begins to collect finished product then, and when backflow stopped, collection of finished products finished;
(4) rectifying finishes, and closes thermal oil turnover valve, stops slide valve pump, and the empty valve of open peace is dressed up article.
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| CN113443983A (en) * | 2021-07-30 | 2021-09-28 | 浙江工业大学 | Production method of dimethyl sebacate |
| CN115385790B (en) * | 2022-09-08 | 2023-11-24 | 江苏正丹化学工业股份有限公司 | Synthesis method of tetraoctyl pyromellitate |
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| CN102718672B (en) * | 2012-06-11 | 2016-05-11 | 山东汉兴医药科技有限公司 | Synthetic method of p-hydroxyphenylglycine methyl ester |
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| CN106674009A (en) * | 2017-03-17 | 2017-05-17 | 濮阳市盛源能源科技股份有限公司 | Reaction device for synthetic production of diisooctyl sebacate, and synthetic process method of diisooctyl sebacate |
| CN111875495A (en) * | 2020-08-21 | 2020-11-03 | 苏州拜傲克生物科技有限公司 | Synthetic method of octadecadienecarboxylic acid mono-tert-butyl ester |
| CN113443983A (en) * | 2021-07-30 | 2021-09-28 | 浙江工业大学 | Production method of dimethyl sebacate |
| CN113443983B (en) * | 2021-07-30 | 2022-02-22 | 浙江工业大学 | Production method of dimethyl sebacate |
| CN115385790B (en) * | 2022-09-08 | 2023-11-24 | 江苏正丹化学工业股份有限公司 | Synthesis method of tetraoctyl pyromellitate |
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