CN103936587A - Triacetin preparation method - Google Patents
Triacetin preparation method Download PDFInfo
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- CN103936587A CN103936587A CN201410085667.6A CN201410085667A CN103936587A CN 103936587 A CN103936587 A CN 103936587A CN 201410085667 A CN201410085667 A CN 201410085667A CN 103936587 A CN103936587 A CN 103936587A
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- preparation
- glycerine
- tubular reactor
- insulation reaction
- acetyl chloride
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/14—Preparation of carboxylic acid esters from carboxylic acid halides
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a triacetin preparation method, which comprises that: glycerol and acetyl chloride respectively pass through a graphite tubular reactor, the tubular reactor is cooled by using salt water, a material enters a vapor-liquid separator from the tubular reactor to separate most of hydrogen chloride gas, and then enters a thermal insulation reaction kettle so as to be subjected to a thermal insulation reaction, reduced pressure evaporation is performed to remove the produced hydrogen chloride gas, and a falling film absorber is adopted to absorb the produced hydrochloric acid by-product. The preparation method has characteristics of no requirement of catalyst and water-carrying agent, clean production achieving, low cost, simple process, high product purity, high reaction efficiency and low energy source consumption.
Description
Technical field
The present invention relates to a kind of Field of Fine Chemicals, relate in particular to a kind of preparation method of glycerine triacetate.
Background technology
Glycerine triacetate is a kind of sticky oily liquids of no color or smell, and bitter is nontoxic, nonirritant, and easily degraded, can be miscible with ethanol, ether, chloroform and benzene, is slightly soluble in water and dithiocarbonic anhydride.Mainly be used as cigarette filter binding agent, perfume fixative, solvent and softening agent, light is put industries such as being applied to tobacco, food, ink, makeup, casting, medicine, dyestuff.
At present, the annual requirement of global glycerine triacetate is in 110,000 about t, and actual ultimate production is in 10.8 ten thousand t left and right, and the demand of glycerine triacetate is slightly larger than its actual ultimate production.Along with the continuous expansion of the Application Areas of glycerine triacetate, its demand is estimated the speed increment with annual 5% ~ 10%, and glycerine triacetate is a large fine chemical product with wide Application Areas and bright market prospects.
The synthesis technique of glycerine triacetate is a lot, and (1) generates reacting of glycerine triacetate and sodium-chlor taking glyceryl trichloride and sodium-acetate as raw material in solvent; (2) glycerine and Glacial acetic acid first esterification under catalyst action, then adds the further acidylate of acetic anhydride; (3) glycerine and acetic anhydride directly catalyze and synthesize the method for glycerine triacetate; (4) catalyze and synthesize the method for glycerine triacetate with epoxy chloropropane and Glacial acetic acid.In existing industrial production, use maximum be technique (2), although there is a lot of research to improve to a certain extent productive rate aspect catalyzer, its yield is also difficult to reach more than 90%.And the solvent of having used lower boiling and water azeotropic in this reaction as benzene, toluene, ethyl acetate etc., this has not only increased cost but also because solvent and miscible being difficult to of glycerine triacetate eliminate, this has just caused has the smell of solvent and the toxicity of benzene kind solvent to limit its application in food, makeup, medicine and other fields in product.
Summary of the invention
The object of this invention is to provide a kind of cost low, can avoid using the preparation method of a kind of glycerine triacetate that catalyzer and azeotropic agent and purity are high.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of glycerine triacetate, it is characterized in that: respectively glycerine and Acetyl Chloride 98Min. are passed through to graphite tubular reactor, tubular reactor is lowered the temperature by brine refrigeration, material enters vapour liquid separator from tubular reactor and isolates most of hydrogen chloride gas, then enters insulation reaction still, insulation reaction, remove generation hydrogenchloride under reduced pressure, by falling-film absorber absorption production hydrochloric acid by-product.
In this preparation method, the mol ratio of described glycerine and Acetyl Chloride 98Min. is 1:3 ~ 3.5.
In this preparation method, the mol ratio of described glycerine and Acetyl Chloride 98Min. is 1:3..2.
In this preparation method, described glycerine and Acetyl Chloride 98Min. are 800 ~ 2000L/h by the overall flow rate of tubular reactor.
In this preparation method, the length-to-diameter ratio of described graphite tubular reactor is 100 ~ 10000.
In this preparation method, the temperature of insulation reaction is 90 ~ 120 DEG C.
In this preparation method, the time of insulation reaction is 1 ~ 5h.
In this preparation method, the pressure that removes hydrogenchloride under reduced pressure is-0.07 ~-0.095MPa.
In this preparation method, respectively by glycerine and Acetyl Chloride 98Min. according to the ratio of mol ratio 1:3.2, by graphite tubular type reactor reaction, control temperature≤35 DEG C of tubular reactor with the speed of total flux 1200L/h; Material enters gas-liquid separator from tubular reactor, isolates most of hydrogen chloride gas; Then enter insulation reaction still, in 110 DEG C of insulation reaction 3h, decompression-0.09MPa steams except hydrogenchloride, by falling-film absorber absorption production hydrochloric acid by-product.
Advantageous effect of the present invention is: due to this preparation method of the present invention, so do not need catalyzer and azeotropic agent, realized cleaner production, cost is low; Technique is simple, and product purity is high; Reaction efficiency is high, and energy consumption is low; Another product of the present invention, without any objectionable impurities, has expanded use range, can be applied to the high-end fields such as food, makeup, medicine.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
Respectively by glycerine and Acetyl Chloride 98Min. according to the ratio of mol ratio 1:3.2, by graphite tubular type reactor reaction, control temperature≤35 DEG C of tubular reactor with the speed of total flux 1200L/h; Material enters gas-liquid separator from tubular reactor, isolates most of hydrogen chloride gas; Then enter insulation reaction still, in 110 DEG C of insulation reaction 3h, decompression-0.09MPa steams except hydrogenchloride, by falling-film absorber absorption production hydrochloric acid by-product.
Embodiment 2
Respectively by glycerine and Acetyl Chloride 98Min. according to the ratio of mol ratio 1:3.0, by graphite tubular type reactor reaction, control temperature≤35 DEG C of tubular reactor with the speed of total flux 1000L/h; Material enters gas-liquid separator from tubular reactor, isolates most of hydrogen chloride gas; Then enter insulation reaction still, in 110 DEG C of insulation reaction 2h, decompression-0.08MPa steams except hydrogenchloride, by falling-film absorber absorption production hydrochloric acid by-product.
Embodiment 3
Respectively by glycerine and Acetyl Chloride 98Min. according to the ratio of mol ratio 1:3.1, by graphite tubular type reactor reaction, control temperature≤35 DEG C of tubular reactor with the speed of total flux 800L/h; Material enters gas-liquid separator from tubular reactor, isolates most of hydrogen chloride gas; Then enter insulation reaction still, in 100 DEG C of insulation reaction 4h, decompression-0.09MPa steams except hydrogenchloride, by falling-film absorber absorption production hydrochloric acid by-product.
Embodiment 4
Respectively by glycerine and Acetyl Chloride 98Min. according to the ratio of mol ratio 1:3.5, by graphite tubular type reactor reaction, control temperature≤35 DEG C of tubular reactor with the speed of total flux 1500L/h; Material enters gas-liquid separator from tubular reactor, isolates most of hydrogen chloride gas; Then enter insulation reaction still, in 90 DEG C of insulation reaction 4h, decompression-0.09MPa steams except hydrogenchloride, by falling-film absorber absorption production hydrochloric acid by-product.
The invention discloses a kind of Acetyl Chloride 98Min. of using as acylating reagent, without the reaction process of catalyzer and azeotropic agent.Violent for fear of Acetyl Chloride 98Min. and glycerine reaction heat release, the present invention utilizes graphite tubular reactor, and the heat of the large generation of specific surface area can shift very soon.Then shift entering insulation reaction still and improve temperature and fully react, steam and obtain the high purity glycerine triacetate of purity > 99% except hydrogenchloride.
Claims (9)
1. the preparation method of a glycerine triacetate, it is characterized in that: respectively glycerine and Acetyl Chloride 98Min. are passed through to graphite tubular reactor, tubular reactor is lowered the temperature by brine refrigeration, material enters vapour liquid separator from tubular reactor and isolates most of hydrogen chloride gas, then enter insulation reaction still, insulation reaction, removes generation hydrogenchloride under reduced pressure, by falling-film absorber absorption production hydrochloric acid by-product.
2. the preparation method of a kind of glycerine triacetate according to claim 1, is characterized in that: the mol ratio of described glycerine and Acetyl Chloride 98Min. is 1:3 ~ 3.5.
3. the preparation method of a kind of glycerine triacetate according to claim 2, is characterized in that: the mol ratio of described glycerine and Acetyl Chloride 98Min. is 1:3..2.
4. the preparation method of a kind of glycerine triacetate according to claim 3, is characterized in that: described glycerine and Acetyl Chloride 98Min. are 800 ~ 2000L/h by the overall flow rate of tubular reactor.
5. the preparation method of a kind of glycerine triacetate according to claim 4, is characterized in that: the length-to-diameter ratio of described graphite tubular reactor is 100～10000.
6. the preparation method of a kind of glycerine triacetate according to claim 5, is characterized in that: the temperature of insulation reaction is 90 ~ 120 DEG C.
7. the preparation method of a kind of glycerine triacetate according to claim 6, is characterized in that: the time of insulation reaction is 1 ~ 5h.
8. the preparation method of a kind of glycerine triacetate according to claim 7, is characterized in that: the pressure that removes hydrogenchloride under reduced pressure is-0.07 ~-0.095MPa.
9. according to the preparation method of a kind of glycerine triacetate described in claim 1 or 7, it is characterized in that: respectively by glycerine and Acetyl Chloride 98Min. according to the ratio of mol ratio 1:3.2, speed with total flux 1200L/h is passed through graphite tubular type reactor reaction, controls temperature≤35 DEG C of tubular reactor; Material enters gas-liquid separator from tubular reactor, isolates most of hydrogen chloride gas; Then enter insulation reaction still, in 110 DEG C of insulation reaction 3h, decompression-0.09MPa steams except hydrogenchloride, by falling-film absorber absorption production hydrochloric acid by-product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410085667.6A CN103936587A (en) | 2014-03-11 | 2014-03-11 | Triacetin preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410085667.6A CN103936587A (en) | 2014-03-11 | 2014-03-11 | Triacetin preparation method |
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| CN103936587A true CN103936587A (en) | 2014-07-23 |
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| CN201410085667.6A Pending CN103936587A (en) | 2014-03-11 | 2014-03-11 | Triacetin preparation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677497A (en) * | 2022-11-01 | 2023-02-03 | 上海橡实化学有限公司 | Production method of ethyl benzoate |
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2014
- 2014-03-11 CN CN201410085667.6A patent/CN103936587A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677497A (en) * | 2022-11-01 | 2023-02-03 | 上海橡实化学有限公司 | Production method of ethyl benzoate |
| CN115677497B (en) * | 2022-11-01 | 2024-05-14 | 山东华泰新材料技术研发有限公司 | Production method of ethyl benzoate |
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Application publication date: 20140723 |