CN105085456A - High-pressure chlorination hydrolysis method in ethyl maltol continuous production - Google Patents
High-pressure chlorination hydrolysis method in ethyl maltol continuous production Download PDFInfo
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- CN105085456A CN105085456A CN201510517558.1A CN201510517558A CN105085456A CN 105085456 A CN105085456 A CN 105085456A CN 201510517558 A CN201510517558 A CN 201510517558A CN 105085456 A CN105085456 A CN 105085456A
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- pressure
- kettle
- temperature
- distillation
- chlorinating container
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
Abstract
The invention discloses a high-pressure chlorination hydrolysis method in ethyl maltol continuous production, which comprises the following steps: connecting an overflow port of a chlorination reaction kettle to a high-pressure reaction kettle to introduce steam to heat the high-pressure reaction kettle, reacting for 2.5 hours while controlling the temperature in the kettle at 120-135 DEG C and the pressure at 1-1.5 MPa, closing the steam valve, starting circulating water to cool the inside of the kettle to 80 DEG C, and recovering methyl chloride gas; when the pressure of the kettle drops to 0.05 MPa, closing the circulating water inlet and outlet, and starting steam distillation to recover unreacted methanol; and after the distillation finishes, starting the circulating water for cooling, adding a small amount of alkali liquor into the kettle to regulate the pH value to 2.5-3.0, and precipitating the ethyl maltol crude product. The methanol and hydrochloric acid can react more sufficiently in the high-temperature high-pressure environment to generate more methyl chloride, thereby reducing the existence of acids, reducing the consumption of the alkali liquor for neutralization, reducing the salt content in sewage, lowering the environmental pollution, increasing the methyl chloride yield and greatly enhancing the benefits of the enterprise.
Description
Technical field
The present invention relates to a kind of ethyl maltol chlorination continuous production method, the high pressure chlorination method for hydrolysis particularly in a kind of veltol plus continuous seepage.
Background technology
Chlorination reaction in veltol plus continuous seepage is raw material with chlorine, a large amount of chlorion and acid generation is had in reaction process, veltol plus is the most easily separated out between pH value 2.5-3.0, prior art utilizes hydrolysis kettle to add a large amount of liquid caustic soda to carry out neutralizing unnecessary acid, sodium ion in liquid caustic soda and chloride binding generate salt, make saltiness in sewage very high, be difficult to process, cause serious environmental pollution.
Summary of the invention
The invention provides the high pressure chlorination method for hydrolysis in a kind of veltol plus continuous seepage, by reducing the amount of unnecessary acid, reaching and reducing liquid caustic soda consumption, reduce the object of saltiness in sewage, methyl chloride output can be increased simultaneously, greatly improve enterprise's productivity effect.
The object of the invention is to be achieved by the following technical programs, high pressure chlorination method for hydrolysis in a kind of veltol plus continuous seepage, comprise the methanol solution squeezing into recovery to chlorinating container, chlorinating container opens outer circulation refrigeration, in chlorinating container, furfuryl alcohol is dripped continuously when methanol solution temperature is down to-10 DEG C, passing into chlorine continuously carries out chlorination reaction simultaneously, reaction heat is exchanged by outer cold heat exchanger by recycle pump, it is characterized in that, the overflow port of chlorinating container connects autoclave, when the liquid level in chlorinating container is increased to overflow port, automatic overflow is to autoclave, draw steam heating autoclave, temperature in the kettle controls at 120-135 DEG C, pressure-controlling is at 1-1.5Mpa, react after 2.5 hours, steam off valve, open cycle water for cooling, when temperature in the kettle is down to 80 DEG C, slow unlatching pressure release valve, reclaim methyl chloride gas, when still pressure drop is to 0.05Mpa, closedown recirculated water is imported and exported, open vapor distillation and reclaim unreacted methyl alcohol, distillation terminates rear open cycle water for cooling, in still, add a small amount of alkali lye makes pH value be adjusted between 2.5-3.0, separate out veltol plus crude product.
Preferably, the distillation temperature reclaiming unreacted methanol controls between 90-95 DEG C, and distillation time is 3-4 hours.
Beneficial effect: the present invention abandons prior art and utilizes chlorinated hydrolysis still to be hydrolyzed, material in chlorinating container directly enters autoclave through overflow port, by regulating temperature and pressure in autoclave, methyl alcohol and hydrochloric acid react more abundant under the environment of High Temperature High Pressure, generate more methyl chloride, the existence of acid will be greatly reduced like this, reduce the usage quantity of next step alkali lye, reduce saltiness in sewage, reduce environmental pollution, add methyl chloride output simultaneously, greatly improve enterprise's productivity effect.
Embodiment
High pressure chlorination method for hydrolysis in a kind of veltol plus continuous seepage, comprise the methanol solution squeezing into recovery to chlorinating container, chlorinating container opens outer circulation refrigeration, in chlorinating container, furfuryl alcohol is dripped continuously when methanol solution temperature is down to-10 DEG C, passing into chlorine continuously carries out chlorination reaction simultaneously, reaction heat is exchanged by outer cold heat exchanger by recycle pump, the overflow port of chlorinating container connects autoclave, when the liquid level in chlorinating container is increased to overflow port, automatic overflow is in autoclave; Opening steam heating makes temperature in the kettle rise to 120-135 DEG C, and still internal pressure controls at 1-1.5Mpa; Then insulation reaction is after 2.5 hours, steam off valve, open cycle water for cooling 2.5 hours; When still temperature drop to 80 DEG C, slowly open pressure release valve, reclaim methyl chloride gas, when still pressure drop is to 0.05Mpa, closes recirculated water and import and export, open vapor distillation and reclaim unreacted methyl alcohol.Distillation temperature finally controls between 90 ~ 95 DEG C, and distillation time is 3.5 hours; Distillation terminates rear open cycle water for cooling, adds a small amount of alkali lye and make pH value be adjusted between 2.5 ~ 3.0 in still, separates out veltol plus crude product.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (2)
1. the high pressure chlorination method for hydrolysis in a veltol plus continuous seepage, comprise the methanol solution squeezing into recovery to chlorinating container, chlorinating container opens outer circulation refrigeration, in chlorinating container, furfuryl alcohol is dripped continuously when methanol solution temperature is down to-10 DEG C, passing into chlorine continuously carries out chlorination reaction simultaneously, reaction heat is exchanged by outer cold heat exchanger by recycle pump, it is characterized in that, the overflow port of chlorinating container connects autoclave, when the liquid level in chlorinating container is increased to overflow port, automatic overflow is to autoclave, draw steam heating autoclave, temperature in the kettle controls at 120-135 DEG C, pressure-controlling is at 1-1.5Mpa, react after 2.5 hours, steam off valve, open cycle water for cooling, when temperature in the kettle is down to 80 DEG C, slow unlatching pressure release valve, reclaim methyl chloride gas, when still pressure drop is to 0.05Mpa, closedown recirculated water is imported and exported, open vapor distillation and reclaim unreacted methyl alcohol, distillation terminates rear open cycle water for cooling, in still, add a small amount of alkali lye makes pH value be adjusted between 2.5-3.0, separate out veltol plus crude product.
2. the high pressure chlorination method for hydrolysis according to claim 1 in a kind of veltol plus continuous seepage, is characterized in that, the distillation temperature reclaiming unreacted methanol controls between 90-95 DEG C, and distillation time is 3-4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517558.1A CN105085456A (en) | 2015-08-22 | 2015-08-22 | High-pressure chlorination hydrolysis method in ethyl maltol continuous production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510517558.1A CN105085456A (en) | 2015-08-22 | 2015-08-22 | High-pressure chlorination hydrolysis method in ethyl maltol continuous production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105085456A true CN105085456A (en) | 2015-11-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510517558.1A Pending CN105085456A (en) | 2015-08-22 | 2015-08-22 | High-pressure chlorination hydrolysis method in ethyl maltol continuous production |
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| CN (1) | CN105085456A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349204A (en) * | 2016-08-30 | 2017-01-25 | 安徽金禾实业股份有限公司 | Neutralization method for chlorination-hydrolysis during production of maltol |
| CN114369077A (en) * | 2022-02-10 | 2022-04-19 | 河北省天利海香精香料有限公司 | Neutralization method of ethyl maltol |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4342697A (en) * | 1975-08-28 | 1982-08-03 | Pfizer Inc. | Preparation of gamma-pyrones |
| US4387235A (en) * | 1979-09-04 | 1983-06-07 | Pfizer Inc. | Intermediates for the preparation of gamma-pyrones |
| CN101585822A (en) * | 2009-06-26 | 2009-11-25 | 滁州学院 | Ethyl maltol synthetic method |
| CN102391229A (en) * | 2011-09-07 | 2012-03-28 | 安徽金禾实业股份有限公司 | Ethyl maltol chlorination continuous production method and device |
| CN104341378A (en) * | 2014-09-27 | 2015-02-11 | 安徽金禾实业股份有限公司 | Chlorination hydrolysis production method in ethyl maltol production |
-
2015
- 2015-08-22 CN CN201510517558.1A patent/CN105085456A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4342697A (en) * | 1975-08-28 | 1982-08-03 | Pfizer Inc. | Preparation of gamma-pyrones |
| US4387235A (en) * | 1979-09-04 | 1983-06-07 | Pfizer Inc. | Intermediates for the preparation of gamma-pyrones |
| CN101585822A (en) * | 2009-06-26 | 2009-11-25 | 滁州学院 | Ethyl maltol synthetic method |
| CN102391229A (en) * | 2011-09-07 | 2012-03-28 | 安徽金禾实业股份有限公司 | Ethyl maltol chlorination continuous production method and device |
| CN104341378A (en) * | 2014-09-27 | 2015-02-11 | 安徽金禾实业股份有限公司 | Chlorination hydrolysis production method in ethyl maltol production |
Non-Patent Citations (1)
| Title |
|---|
| 董立涛: "麦芽酚、乙基麦芽酚及其在食品工业中的应用", 《食品工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349204A (en) * | 2016-08-30 | 2017-01-25 | 安徽金禾实业股份有限公司 | Neutralization method for chlorination-hydrolysis during production of maltol |
| CN114369077A (en) * | 2022-02-10 | 2022-04-19 | 河北省天利海香精香料有限公司 | Neutralization method of ethyl maltol |
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Application publication date: 20151125 |
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