CN108355372B - Method and device for sublimating and receiving maltol - Google Patents
Method and device for sublimating and receiving maltol Download PDFInfo
- Publication number
- CN108355372B CN108355372B CN201810038451.2A CN201810038451A CN108355372B CN 108355372 B CN108355372 B CN 108355372B CN 201810038451 A CN201810038451 A CN 201810038451A CN 108355372 B CN108355372 B CN 108355372B
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- kettle
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Soy Sauces And Products Related Thereto (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention relates to a method for sublimating and receiving maltol, which comprises the following steps: a. sublimed steam at the temperature of 160-220 ℃ from the subliming kettle enters an inlet at the upper part of the horizontal receiving kettle, and under the stirring of a multi-stage rotary stirrer in the horizontal receiving kettle, steam materials are fully contacted and absorbed with cooling water in the kettle, and meanwhile, the temperature of the absorbing liquid in the horizontal receiving kettle is controlled to be 70-80 ℃ by the cooling water; b. the unabsorbed steam material enters a secondary vertical receiving kettle from an outlet at the upper part of the horizontal receiving kettle, and a jacket outside the vertical receiving kettle adopts saline water at the temperature of-12 ℃ to-15 ℃ to carry out conventional absorption on the steam material in the kettle. The horizontal receiving kettle is adopted, so that the residence time of the sublimed materials in the receiving kettle is prolonged, the material receiving capacity is improved, the number of equipment is reduced, the stability of the vacuum degree is maintained, the aim of enhancing the sublimed receiving sedimentation is fulfilled, the production yield is improved, and the horizontal receiving kettle has greater economic benefit.
Description
Technical Field
The production process of maltol is divided into a Grignard working section, a chlorination working section, a sublimation working section, a crystallization working section and a drying working section. The sublimation working section has low yield all the time, and the main reason is that the sublimation receiving device is too traditional, a vertical reaction kettle type three-stage receiving mode is adopted in production, materials are rapidly fed in and discharged out, the heat exchange efficiency is poor, great limitation is caused to production, and a large amount of products are still carried out at a tail gas outlet; and the receiving links are too many, the vacuum degree is difficult to control, the sublimation rate is influenced, partial materials are heated and decomposed into byproducts for a long time, and the product quality and the yield are seriously influenced.
Disclosure of Invention
The invention aims to solve the defects of low efficiency and poor product quality of a sublimation receiving device in the prior art, and provides the sublimation receiving device for maltol.
The technical scheme adopted by the invention is as follows:
1. a method for sublimation reception of maltol, characterized by comprising the steps of:
a. sublimed steam at the temperature of 160-220 ℃ from the subliming kettle enters an inlet at the upper part of the horizontal receiving kettle, and under the stirring of a multi-stage rotary stirrer in the horizontal receiving kettle, steam materials are fully contacted and absorbed with cooling water in the kettle, and meanwhile, the temperature of the absorbing liquid in the horizontal receiving kettle is controlled to be 70-80 ℃ by the cooling water;
b. the unabsorbed steam material enters a secondary vertical receiving kettle from an outlet at the upper part of the horizontal receiving kettle, and a jacket outside the vertical receiving kettle adopts saline water at the temperature of-12 ℃ to-15 ℃ to carry out conventional absorption on the steam material in the kettle.
2. The utility model provides a realize device of sublimation receiving method of maltol which characterized in that passes through the pipe connection by sublimation cauldron, horizontal receiving kettle and vertical receiving kettle and constitutes, and its characterized in that horizontal receiving kettle includes: the horizontal round kettle body is provided with a horizontal stirring shaft and a motor connected with the horizontal stirring shaft in the center, the stirring shaft is provided with a group of spiral stirrers, and two ends of the round kettle body are respectively provided with a material inlet and a material outlet.
The horizontal receiving kettle has the advantages that the horizontal receiving kettle is adopted, the retention time of the sublimed materials in the receiving kettle is mainly prolonged, the heat exchange between the materials and a liquid phase can be more sufficient, the capacity of receiving the materials is greatly improved, the number of equipment is reduced, and the stability of the vacuum degree is maintained. By using the novel receiving device, the vacuum cooling condition is not affected, the aim of strengthening sublimation receiving sedimentation is achieved, the production yield is improved, and the economic benefit is greater.
Drawings
FIG. 1 is a system flow diagram of the present invention;
FIG. 2 is a block diagram of the horizontal receiver tank of FIG. 1.
Detailed Description
The device for realizing the sublimation receiving method of maltol provided by the invention comprises a sublimation kettle, a horizontal receiving kettle and a vertical receiving kettle which are connected through a pipeline, wherein the horizontal receiving kettle comprises: horizontal circular cauldron body 1, circular cauldron body center are equipped with horizontal (mixing) shaft 4 and continuous motor 5, are equipped with a set of spiral agitator 3 on the (mixing) shaft, and circular cauldron body both ends are equipped with material import and material export respectively, are equipped with on the circular cauldron body and press from both sides cover 2, and the upper and lower end that presss from both sides cover 2 is equipped with the refrigerant respectively and imports and exports, and circular cauldron body one side bottom is equipped with the baiting valve. The circular kettle body is connected to a bracket 6.
Secondly, as shown in fig. 1 and fig. 2, the invention provides a sublimation receiving method of maltol,
1. the method is mainly applied to the condensation of a maltol sublimation post for receiving materials, the crude maltol generated by the reaction contains a large amount of asphalt by-products, and in order to primarily separate the products, a decompression sublimation mode is adopted; the system material comes from chlorination hydrolysis reaction process after, two cauldron black oil that the formation of hydrolysising put into a sublimation cauldron and carry out the sublimation, black oil volume is about 1 cube, and the sublimation cauldron is 1.5 cubes, and horizontal acceptance kettle is 2 cubes.
2. Putting the materials into a sublimation kettle, stirring, jacket oil heating, starting a vacuum pump when the temperature in the kettle rises to about 160 ℃, ensuring that the vacuum degree is not lower than-0.8 MPa, starting stirring at a water distribution 1 side of a horizontal receiving kettle, starting sublimation, adjusting the oil temperature (the oil temperature is not higher than 280 ℃) according to the distillation yield of the receiving kettle, gradually raising the kettle temperature along with the sublimation of maltol, sublimating for 4 hours until the kettle rises to 230-240 ℃, observing the state of residual asphalt in the kettle, and judging the sublimation end point to discharge asphalt.
3. Sublimed steam at the temperature of 160-220 ℃ from the subliming kettle enters an inlet at the upper part of the horizontal receiving kettle, and under the stirring of a multi-stage rotary stirrer 4 in the horizontal receiving kettle, the steam material is fully contacted with cooling water in the kettle for absorption, and meanwhile, the temperature of the absorption liquid in the jacket 2 for the horizontal receiving kettle is controlled to be 70-80 ℃; the unabsorbed steam material enters a secondary vertical receiving kettle from an outlet at the upper part of the horizontal receiving kettle, and a jacket outside the vertical receiving kettle adopts saline water at the temperature of-12 ℃ to-15 ℃ to carry out conventional absorption on the steam material in the kettle.
The invention changes the first receiving kettle into a horizontal receiving device, and mainly improves the following steps: 1) the residence time of the high-temperature materials in the receiving device is prolonged, 2) the multistage stirring can better drive the device to exchange heat with the cooling water of the high-temperature materials, the sedimentation effect is improved, 3) the materials are settled in time, the vacuum compensation is not performed, the vacuum degree is obviously improved, the acting effect of a vacuum pump is better, and 4) the original receiving kettle has three stages, namely, one kettle in the 2 directions and 2 kettles in the 1 direction; now improved to a 2-squareHorizontal type Receiving kettleAnd a receiving kettle of the 1 part can meet the production requirement. 4. The improvement of the vacuum kettle reduces the sublimation temperature, shortens the sublimation time, reduces the high-temperature decomposition of materials, improves the yield of a single kettle, reduces the introduction of high-boiling-point impurities into a receiving kettle, and has better product quality; can sublime thorough pitch pairThe product is not easy to wrap materials, and the amount of the asphalt which is a byproduct of a single kettle is little.
Claims (2)
1. A sublimation receiving method of maltol black oil, which is characterized by comprising the following steps:
a, allowing sublimation steam at 220 ℃ from a sublimation kettle to enter an inlet at the upper part of the horizontal receiving kettle, and allowing the steam material to be fully contacted and absorbed with cooling water in the kettle under the stirring of a multi-stage rotary stirrer in the horizontal receiving kettle, wherein the temperature of the absorption liquid in the horizontal receiving kettle is controlled to be 70-80 ℃ by using the cooling water;
and b, allowing unabsorbed steam materials to enter a secondary vertical receiving kettle from an outlet at the upper part of the horizontal receiving kettle, and conventionally absorbing the steam materials in the kettle by using saline water at the temperature of-12 ℃ to-15 ℃ through a jacket outside the vertical receiving kettle.
2. The utility model provides a realize device of sublimation receiving method of maltol black oil which characterized in that passes through the pipe connection by sublimation cauldron, horizontal receipt cauldron and vertical receipt cauldron and constitutes, and its characterized in that horizontal receipt cauldron includes: the horizontal round kettle (1) is characterized in that a horizontal stirring shaft (4) and a motor (5) connected with the horizontal stirring shaft are arranged at the center of the round kettle, a group of spiral stirrers (3) are arranged on the stirring shaft, a material inlet and a material outlet are respectively arranged at two ends of the round kettle, a jacket (2) is arranged on the round kettle, and a refrigerant inlet and a refrigerant outlet are respectively arranged at the upper end and the lower end of the jacket (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810038451.2A CN108355372B (en) | 2018-01-13 | 2018-01-13 | Method and device for sublimating and receiving maltol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810038451.2A CN108355372B (en) | 2018-01-13 | 2018-01-13 | Method and device for sublimating and receiving maltol |
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| Publication Number | Publication Date |
|---|---|
| CN108355372A CN108355372A (en) | 2018-08-03 |
| CN108355372B true CN108355372B (en) | 2020-09-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810038451.2A Active CN108355372B (en) | 2018-01-13 | 2018-01-13 | Method and device for sublimating and receiving maltol |
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| Country | Link |
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| CN (1) | CN108355372B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535113A (en) * | 2018-12-10 | 2019-03-29 | 安徽金禾实业股份有限公司 | A kind of maltol lyophilization method and device |
| CN109503536A (en) * | 2018-12-10 | 2019-03-22 | 安徽金禾实业股份有限公司 | A kind of ethylmaltol method of purification and device |
| CN112742061A (en) | 2020-12-11 | 2021-05-04 | 安徽金禾实业股份有限公司 | Cooling device and cooling method for maltol sublimation section |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2135394Y (en) * | 1992-09-15 | 1993-06-09 | 曹丽娜 | Water absorption chamber |
| CA2259481A1 (en) * | 1998-02-09 | 1999-08-09 | Kemestrie Inc. | Direct extraction and/or purification of high purity maltol and essential oils by sublimation process |
| CN101993428A (en) * | 2010-11-10 | 2011-03-30 | 广东省肇庆香料厂有限公司 | Method for purifying ethyl maltol |
| CN103113339A (en) * | 2012-11-11 | 2013-05-22 | 安徽金禾实业股份有限公司 | Maltol separation and purification method |
| CN106310700A (en) * | 2015-07-08 | 2017-01-11 | 陕西天汉生物科技有限公司 | Ethyl maltol crystallization sublimation process capable of reducing energy consumption |
-
2018
- 2018-01-13 CN CN201810038451.2A patent/CN108355372B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2135394Y (en) * | 1992-09-15 | 1993-06-09 | 曹丽娜 | Water absorption chamber |
| CA2259481A1 (en) * | 1998-02-09 | 1999-08-09 | Kemestrie Inc. | Direct extraction and/or purification of high purity maltol and essential oils by sublimation process |
| CN101993428A (en) * | 2010-11-10 | 2011-03-30 | 广东省肇庆香料厂有限公司 | Method for purifying ethyl maltol |
| CN103113339A (en) * | 2012-11-11 | 2013-05-22 | 安徽金禾实业股份有限公司 | Maltol separation and purification method |
| CN106310700A (en) * | 2015-07-08 | 2017-01-11 | 陕西天汉生物科技有限公司 | Ethyl maltol crystallization sublimation process capable of reducing energy consumption |
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| CN108355372A (en) | 2018-08-03 |
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