CN112409304A - Purification method of intermediate in Grignard section of maltol - Google Patents

Purification method of intermediate in Grignard section of maltol Download PDF

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Publication number
CN112409304A
CN112409304A CN202011442706.5A CN202011442706A CN112409304A CN 112409304 A CN112409304 A CN 112409304A CN 202011442706 A CN202011442706 A CN 202011442706A CN 112409304 A CN112409304 A CN 112409304A
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flash evaporation
evaporation kettle
stage flash
temperature
kettle
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CN202011442706.5A
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詹见
陈金林
谢国柱
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Anhui Jinhe Industrial Co Ltd
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Anhui Jinhe Industrial Co Ltd
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Priority to CN202011442706.5A priority Critical patent/CN112409304A/en
Publication of CN112409304A publication Critical patent/CN112409304A/en
Priority to PCT/CN2021/137217 priority patent/WO2022122030A1/en
Priority to CN202180065858.4A priority patent/CN116261559A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
    • C07D307/40—Radicals substituted by oxygen atoms
    • C07D307/42—Singly bound oxygen atoms
    • C07D307/44—Furfuryl alcohol
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A method for purifying a maltol Grignard section intermediate comprises the following steps: the intermediate has a molar mass of 2m3The flow of the gas enters a rectifying tower at the bottom temperature of 60 ℃ and the top temperature of 40 ℃; then enters a first-stage flash evaporation kettle, and the extraction flow is 1.5m3The temperature of the first-stage flash evaporation kettle is 85 ℃, the gas phase of the first-stage flash evaporation kettle is condensed and then enters a second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 ℃, the gas phase of the second-stage flash evaporation kettle is condensed and then enters a third-stage flash evaporation kettle, the temperature of the third-stage flash evaporation kettle is 60 ℃, the gas phase of the third-stage flash evaporation kettle is condensed and then collected, the flash evaporation kettle is subjected to reduced pressure distillation, and the vacuum degree is-0; returning the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle to the first-stage flash evaporation kettle every 3 hours; 0.5m from the bottom of the first-stage flash evaporation kettle3Qualified furfuryl alcohol is extracted at a flow rate of/h. The method can improve furfuryl alcohol content and yield, and can reduce labor intensity.

Description

Purification method of intermediate in Grignard section of maltol
Technical Field
The invention relates to a method for purifying an intermediate of a maltol Grignard section.
Background
In the production process of maltol, a traditional furfural method is adopted, a grignard reagent reacts with furfural in a toluene and tetrahydrofuran solvent to generate a furfuryl alcohol intermediate, and then a reduced pressure distillation method is adopted to separate the solvent in a reduced pressure distillation kettle to purify furfuryl alcohol. The furfuryl alcohol is used in the chlorination section. The separation and purification method is an intermittent single-kettle operation, and not only has complex operation, low production capacity and high energy consumption, but also has low furfuryl alcohol content and more impurities after purification. The recovered solvent also contains furfuryl alcohol. Resulting in low furfuryl alcohol yield and low quality. The yield and yield of maltol are seriously affected.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for purifying an intermediate in a maltol Grignard section, which can improve the furfuryl alcohol content and yield, solve intermittent repeated operation and reduce the labor intensity of personnel.
The invention provides a method for purifying an intermediate of a maltol Grignard section to solve the technical problem, which is characterized by comprising the following steps:
(1) the intermediate has a molar mass of 2m3The flow of the furfuryl alcohol and the solvent enters a rectifying tower at a flow rate of/h for coarse separation, wherein the tower bottom temperature of the rectifying tower is 60 ℃, and the tower top temperature is 40 ℃;
(2) then the mixture is extracted from the bottom of the rectifying tower and enters a first-stage flash evaporation kettle, and the extraction flow is 1.5m3The temperature of the first-stage flash evaporation kettle is 85 ℃, the gas phase of the first-stage flash evaporation kettle is condensed and then enters a second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 ℃, the gas phase of the second-stage flash evaporation kettle is condensed and then enters a third-stage flash evaporation kettle, the temperature of the third-stage flash evaporation kettle is 60 ℃, the gas phase of the third-stage flash evaporation kettle is condensed and then collected, the temperature of a freezing medium of the gas phase condensation ranges from-5 ℃ to-8 ℃, all the flash evaporation kettles are subjected to reduced pressure distillation, and the vacuum;
(3) returning the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle to the first-stage flash evaporation kettle every 3 hours;
(4) 0.5m from the bottom of the first-stage flash evaporation kettle3Qualified furfuryl alcohol is extracted at a flow rate of/h, and the content of the extracted furfuryl alcohol is analyzed once per hour.
And (2) recycling the solvent separated in the step (1) for production.
And (3) the solvent obtained after gas phase condensation of the third-stage flash evaporation kettle in the step (2) is used for washing magnesium slag in production.
For the sake of simplicity of explanation, the purification method of the intermediate of the maltol grignard section according to the present invention is hereinafter simply referred to as the present method.
The method has the advantages that: the invention realizes continuous production, has strong operability, reduces consumption and improves the yield and quality of the furfuryl alcohol. Plays a decisive role in improving the yield of the whole maltol product.
1. The furfuryl alcohol content is improved from 91 percent to 95 percent.
2. The yield of the furfuryl alcohol reduced by a single kettle is improved from 960kg to 980 kg.
3. The solvent consumption is reduced, the cost is reduced, and 300 liters of the solvent is recycled more per day on average.
4. The continuous production is realized, the labor intensity is reduced, and the production control is more stable.
Drawings
FIG. 1 is a flow chart of the method.
Detailed Description
Referring to fig. 1, the corresponding apparatus of the method comprises a rectifying tower 1, a first flash evaporation kettle 41, a second flash evaporation kettle 42, a third flash evaporation kettle 43, a first condenser 21, a second condenser 22, a third condenser 23, a fourth condenser 24, a first pump 51, a second pump 52, a first solvent tank 31, a second solvent tank 32, and a furfuryl alcohol tank 33, wherein a reboiler 11 is arranged beside the rectifying tower 1 and connected with the rectifying tower 1 through a circulation pipeline, an upper outlet of the rectifying tower 1 is connected with the first condenser 21, the other end of the first condenser 21 is connected with the first solvent tank 31, a lower outlet of the rectifying tower 1 is connected with an inlet of the first flash evaporation kettle 41 through the first pump 51, a lower outlet of the first flash evaporation kettle is connected with the furfuryl alcohol tank 33, an upper outlet of the first flash evaporation kettle 41 is connected with the second condenser 22, the other end of the second condenser 22 is connected with an inlet of the second flash evaporation kettle 42, an upper outlet of the second flash evaporation kettle 42 is connected with the third flash evaporation kettle 23, the other end of the third condenser 23 is connected with the inlet end of the third flash evaporation kettle 43, the upper outlet of the third flash evaporation kettle 43 is connected with the fourth condenser 24, the other end of the fourth condenser 24 is connected with the second solvent tank 32, the lower outlet of the second flash evaporation kettle 42 is combined with the lower outlet of the third flash evaporation kettle 43, and is connected with the inlet end of the first flash evaporation kettle 41 through the second pump 52.
The first embodiment is as follows:
a method for purifying an intermediate of a maltol Grignard section is characterized by comprising the following steps:
(1) the intermediate has a molar mass of 2m3The flow of the furfuryl alcohol and the solvent enters a rectifying tower at a flow rate of/h for coarse separation, wherein the tower bottom temperature of the rectifying tower is 60 ℃, and the tower top temperature is 40 ℃;
(2) then the mixture is extracted from the bottom of the rectifying tower and enters a first-stage flash evaporation kettle, and the extraction flow is 1.5m3The temperature of the first-stage flash evaporation kettle is 85 ℃, the gas phase of the first-stage flash evaporation kettle is condensed and then enters a second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 ℃, the gas phase of the second-stage flash evaporation kettle is condensed and then enters a third-stage flash evaporation kettle, the temperature of the third-stage flash evaporation kettle is 60 ℃, the gas phase of the third-stage flash evaporation kettle is condensed and then collected, the temperature of a freezing medium of the gas phase condensation is-5 ℃, all the flash evaporation kettles are subjected to reduced pressure distillation, and the vacuum degree;
(3) returning the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle to the first-stage flash evaporation kettle every 3 hours;
(4) 0.5m from the bottom of the first-stage flash evaporation kettle3Qualified furfuryl alcohol is extracted at a flow rate of/h, and the content of the extracted furfuryl alcohol is analyzed once per hour.
Example two:
a method for purifying an intermediate of a maltol Grignard section is characterized by comprising the following steps:
(1) the intermediate has a molar mass of 2m3The flow of the furfuryl alcohol and the solvent enters a rectifying tower at a flow rate of/h for coarse separation, wherein the tower bottom temperature of the rectifying tower is 60 ℃, and the tower top temperature is 40 ℃;
(2) then the mixture is extracted from the bottom of the rectifying tower and enters a first-stage flash evaporation kettle, and the extraction flow is 1.5m3The temperature of the first-stage flash evaporation kettle is 85 ℃, the gas phase of the first-stage flash evaporation kettle is condensed and then enters a second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 ℃, the gas phase of the second-stage flash evaporation kettle is condensed and then enters a third-stage flash evaporation kettle, the temperature of the third-stage flash evaporation kettle is 60 ℃, the gas phase of the third-stage flash evaporation kettle is condensed and then collected, the temperature of a freezing medium of the gas phase condensation is-6.5 ℃, all the flash evaporation kettles are subjected to reduced pressure distillation, and the vacuum degree;
(3) returning the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle to the first-stage flash evaporation kettle every 3 hours;
(4) from one toThe bottom of the stage flash evaporation kettle is 0.5m3Qualified furfuryl alcohol is extracted at a flow rate of/h, and the content of the extracted furfuryl alcohol is analyzed once per hour.
Example three:
a method for purifying an intermediate of a maltol Grignard section is characterized by comprising the following steps:
(1) the intermediate has a molar mass of 2m3The flow of the furfuryl alcohol and the solvent enters a rectifying tower at a flow rate of/h for coarse separation, wherein the tower bottom temperature of the rectifying tower is 60 ℃, and the tower top temperature is 40 ℃;
(2) then the mixture is extracted from the bottom of the rectifying tower and enters a first-stage flash evaporation kettle, and the extraction flow is 1.5m3The temperature of the first-stage flash evaporation kettle is 85 ℃, the gas phase of the first-stage flash evaporation kettle is condensed and then enters a second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 ℃, the gas phase of the second-stage flash evaporation kettle is condensed and then enters a third-stage flash evaporation kettle, the temperature of the third-stage flash evaporation kettle is 60 ℃, the gas phase of the third-stage flash evaporation kettle is condensed and then collected, the temperature of a freezing medium of the gas phase condensation is-8 ℃, all the flash evaporation kettles are subjected to reduced pressure distillation, and the vacuum degree;
(3) returning the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle to the first-stage flash evaporation kettle every 3 hours;
(4) 0.5m from the bottom of the first-stage flash evaporation kettle3Qualified furfuryl alcohol is extracted at a flow rate of/h, and the content of the extracted furfuryl alcohol is analyzed once per hour.

Claims (1)

1. A method for purifying an intermediate of a maltol Grignard section is characterized by comprising the following steps:
(1) the intermediate has a molar mass of 2m3The flow of the furfuryl alcohol and the solvent enters a rectifying tower at a flow rate of/h for coarse separation, wherein the tower bottom temperature of the rectifying tower is 60 ℃, and the tower top temperature is 40 ℃;
(2) then the mixture is extracted from the bottom of the rectifying tower and enters a first-stage flash evaporation kettle, and the extraction flow is 1.5m3The temperature of the first-stage flash evaporation kettle is 85 ℃, the gas phase of the first-stage flash evaporation kettle is condensed and then enters the second-stage flash evaporation kettle, the temperature of the second-stage flash evaporation kettle is 65 ℃, the gas phase of the second-stage flash evaporation kettle is condensed and then enters the third-stage flash evaporation kettle, the temperature of the third-stage flash evaporation kettle is 60 ℃, the gas phase of the third-stage flash evaporation kettle is condensed and then collected, and the gas phase is condensedThe temperature of the freezing medium is-5 ℃ to-8 ℃, and all the flash evaporation kettles are subjected to reduced pressure distillation, wherein the vacuum degree is-0.08 MPa;
(3) returning the materials in the second-stage flash evaporation kettle and the third-stage flash evaporation kettle to the first-stage flash evaporation kettle every 3 hours;
(4) 0.5m from the bottom of the first-stage flash evaporation kettle3Qualified furfuryl alcohol is extracted at a flow rate of/h, and the content of the extracted furfuryl alcohol is analyzed once per hour.
CN202011442706.5A 2020-12-11 2020-12-11 Purification method of intermediate in Grignard section of maltol Pending CN112409304A (en)

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CN202011442706.5A CN112409304A (en) 2020-12-11 2020-12-11 Purification method of intermediate in Grignard section of maltol
PCT/CN2021/137217 WO2022122030A1 (en) 2020-12-11 2021-12-10 Method and device for purifying maltol grignard procedure intermediate
CN202180065858.4A CN116261559A (en) 2020-12-11 2021-12-10 Method and device for purifying intermediate in maltol grignard section

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022122030A1 (en) * 2020-12-11 2022-06-16 安徽金禾实业股份有限公司 Method and device for purifying maltol grignard procedure intermediate

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Publication number Priority date Publication date Assignee Title
AU1538300A (en) * 1998-11-24 2000-06-13 University Of Melbourne, The Process for the recovery of low molecular weight phenols, furfural, furfuryl alcohol and/or cellulose or cellulose-rich residues
CN101054368A (en) * 2007-06-06 2007-10-17 济南圣泉集团股份有限公司 Method and apparatus for purification of furfuryl alcohol
JP2009269062A (en) * 2008-05-08 2009-11-19 Gun Ei Chem Ind Co Ltd Binder composition for casting mold making, sand composition for casting mold making, and manufacturing method of casting mold
CN207024668U (en) * 2017-03-02 2018-02-23 山东一诺生物质材料有限公司 A kind of energy saving device in furfuryl alcohol production
CN109020929A (en) * 2018-07-30 2018-12-18 河南心连心化肥有限公司 A kind of crude furfuryl alcohol separator and its separating technology
CN110790732A (en) * 2019-11-19 2020-02-14 安徽金禾实业股份有限公司 Furfuryl alcohol refining and purifying method in maltol production

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US4305790A (en) * 1980-01-31 1981-12-15 Kramer Sr Edward F Multiple effect distillation method and apparatus
CN106542965B (en) * 2016-11-07 2019-07-16 青岛科技大学 The method of low carbon mixed alcohol tower reactor flash separation methanol
CN112409304A (en) * 2020-12-11 2021-02-26 安徽金禾实业股份有限公司 Purification method of intermediate in Grignard section of maltol

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU1538300A (en) * 1998-11-24 2000-06-13 University Of Melbourne, The Process for the recovery of low molecular weight phenols, furfural, furfuryl alcohol and/or cellulose or cellulose-rich residues
CN101054368A (en) * 2007-06-06 2007-10-17 济南圣泉集团股份有限公司 Method and apparatus for purification of furfuryl alcohol
JP2009269062A (en) * 2008-05-08 2009-11-19 Gun Ei Chem Ind Co Ltd Binder composition for casting mold making, sand composition for casting mold making, and manufacturing method of casting mold
CN207024668U (en) * 2017-03-02 2018-02-23 山东一诺生物质材料有限公司 A kind of energy saving device in furfuryl alcohol production
CN109020929A (en) * 2018-07-30 2018-12-18 河南心连心化肥有限公司 A kind of crude furfuryl alcohol separator and its separating technology
CN110790732A (en) * 2019-11-19 2020-02-14 安徽金禾实业股份有限公司 Furfuryl alcohol refining and purifying method in maltol production

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022122030A1 (en) * 2020-12-11 2022-06-16 安徽金禾实业股份有限公司 Method and device for purifying maltol grignard procedure intermediate

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Application publication date: 20210226