CN110981717A - Hydrolysis treatment method for diketene residue - Google Patents
Hydrolysis treatment method for diketene residue Download PDFInfo
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- CN110981717A CN110981717A CN201911381490.3A CN201911381490A CN110981717A CN 110981717 A CN110981717 A CN 110981717A CN 201911381490 A CN201911381490 A CN 201911381490A CN 110981717 A CN110981717 A CN 110981717A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/083—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid anhydrides
- C07C51/087—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid anhydrides by hydrolysis
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/42—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis
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- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for hydrolyzing and treating diketene residues, which aims to solve the problems of low recovery rate of dilute acetic acid and acetone, high Chemical Oxygen Demand (COD) in sewage, high treatment cost and the like in the residue treatment process in the prior art, and provides a method for hydrolyzing and treating diketene residues, wherein the technological conditions of hydrolysis reaction are optimized, the conversion rates of diketene, acetic anhydride and the like in the residues are improved and three hydrolysis reaction tanks are arranged by adjusting temperature, reaction liquid concentration and reaction time, and one of the three hydrolysis reaction tanks is used as a transfer tank, so that continuous feeding of hydrolysis liquid can be realized by rectification; the continuous stable operation of the separation of the hydrolysate is realized through equipment adjustment, an electric valve and the like, the separation efficiency is obviously improved, and the discharge amount and the quality of the acetone and the acetic acid are improved.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for hydrolyzing diketene residue.
Background
The main method for preparing diketene at present is to adopt an acetic acid cracking method, and since diketene belongs to a heat-sensitive substance, insoluble high polymers and self-polymers are easily formed in the synthesis process, and the high polymers form main solid residues in the diketene process. The residue mainly contains acetic anhydride, diketene, etc., and has an offensive odor. The current treatment method for the residues is mainly hydrolysis. The direct products of the hydrolysis reaction of the ketene dimer residue are dilute acetic acid and acetone, and the reaction equation is as follows:
main reaction:
side reaction:
the defects and shortcomings of the prior art are as follows:
the production process of the diketene is basically continuously and automatically controlled, wherein only the hydrolysis reaction of residue treatment belongs to intermittent control, the composition of raw material (diketene residue) components is unstable, the process control is relatively extensive, and the risk coefficient is relatively high. In addition, dilute acetic acid of the current residue hydrolysis product is concentrated and recycled to the diketene product, and acetone can be directly sold in the market; however, the existing process has low recovery rate of dilute acetic acid, low recovery rate of acetone and low content (only 90%), which causes high Chemical Oxygen Demand (COD) in the sewage and high treatment cost.
Disclosure of Invention
In order to solve the problems of low recovery rate of dilute acetic acid and acetone, high Chemical Oxygen Demand (COD) in sewage, high treatment cost and the like in the residue treatment process in the prior art, the invention provides a diketene residue hydrolysis treatment method, which can effectively improve the conversion rate of diketene and acetic anhydride in residues and improve the discharge amount and quality of acetone and acetic acid.
A method for hydrolyzing diketene residue comprises the following specific steps:
first, hydrolysis and dropping operation
1.1: transferring the distillation residues into a residue diluting tank, diluting with the liquid after pumping, and then, pressing the residue in the diluting tank into a high-level tank by using the diluted liquid;
1.2: transferring the dilute acetic acid into a hydrolysis tank, starting the hydrolysis tank to stir, starting interlayer steam, and heating to 70-90 ℃;
1.3: dropwise adding a residue diluent, controlling the temperature of the kettle to be not too high, controlling the temperature of the kettle to be 80-110 ℃ after dropwise adding, and keeping full reflux in the titration reaction process;
1.4: after the dropwise addition, preserving the heat for 2 hours, and transferring the reacted hydrolysate to a transfer tank;
second, continuous separation operation of hydrolysate
2.1: starting a feeding pump, and controlling the feeding flow by adjusting the variable frequency of the feeding pump;
2.2: starting an acetone reflux pump, controlling the temperature of the tower top by controlling the acetone reflux amount, and automatically controlling the reflux amount by the temperature of the tower top;
2.3: the liquid level at the bottom of the tower is set, and the liquid level in the tower is stabilized through an electric V-shaped ball valve, so that the automatic control of the liquid level at the bottom of the tower is realized;
2.4: the steam pressure of the reboiler is set, and the steam regulating valve automatically controls the size of a steam valve according to the set pressure, so that the automatic control of the liquid level of the reboiler is realized;
2.5: setting the temperature of the tower bottom to be between 90 and 110 ℃, automatically adjusting the balance in the stabilizing tower, controlling gas phase discharge through the pressure of a reboiler, setting the pressure of the reboiler, and controlling the discharge amount through the opening of a pressure control regulating valve;
2.6: the liquid level of the reboiler is set, and an electric V-shaped ball valve for controlling the discharge of the residual liquid is used for realizing the automatic adjustment of the liquid level of the reboiler.
The invention has the beneficial effects that: 1. the technological conditions of the hydrolysis reaction are optimized, and the conversion rates of diketene, acetic anhydride and the like in the residues are improved by adjusting the temperature, the concentration of the reaction liquid and the reaction time.
2. Three hydrolysis reaction tanks are arranged, wherein one hydrolysis reaction tank is used as a transfer tank, so that the rectification of the hydrolysis liquid can realize continuous feeding.
3. The continuous stable operation of the separation of the hydrolysate is realized through equipment adjustment, an electric valve and the like, the separation efficiency is obviously improved, and the discharge amount and the quality of the acetone and the acetic acid are improved.
Detailed Description
Example 1: a method for hydrolyzing diketene residue comprises the following specific steps:
first, hydrolysis and dropping operation
1.1: transferring the distillation residues into a residue diluting tank, diluting with the liquid after pumping, and then, pressing the residue in the diluting tank into a high-level tank by using the diluted liquid;
1.2: transferring the dilute acetic acid into a hydrolysis tank, starting the hydrolysis tank to stir, starting interlayer steam, and heating to 70 ℃;
1.3: dripping residue diluent, controlling the temperature of the kettle to be not too high, controlling the temperature of the kettle to be 80 ℃ after dripping, and keeping full reflux in the titration reaction process;
1.4: after the dropwise addition, preserving the heat for 2 hours, and transferring the reacted hydrolysate to a transfer tank;
second, continuous separation operation of hydrolysate
2.1: starting a feeding pump, and controlling the feeding flow by adjusting the variable frequency of the feeding pump;
2.2: starting an acetone reflux pump, controlling the temperature of the tower top by controlling the acetone reflux amount, and automatically controlling the reflux amount by the temperature of the tower top;
2.3: the liquid level at the bottom of the tower is set, and the liquid level in the tower is stabilized through an electric V-shaped ball valve, so that the automatic control of the liquid level at the bottom of the tower is realized;
2.4: the steam pressure of the reboiler is set, and the steam regulating valve automatically controls the size of a steam valve according to the set pressure, so that the automatic control of the liquid level of the reboiler is realized;
2.5: setting the temperature at the bottom of the tower to be between 90 ℃, automatically adjusting the balance in the stabilizing tower, controlling the gas phase discharge through the pressure of a reboiler, setting the pressure of the reboiler, and controlling the discharge amount through the opening of a pressure control regulating valve;
2.6: the liquid level of the reboiler is set, and an electric V-shaped ball valve for controlling the discharge of the residual liquid is used for realizing the automatic adjustment of the liquid level of the reboiler.
Example 2: a method for hydrolyzing diketene residue comprises the following specific steps:
first, hydrolysis and dropping operation
1.1: transferring the distillation residues into a residue diluting tank, diluting with the liquid after pumping, and then, pressing the residue in the diluting tank into a high-level tank by using the diluted liquid;
1.2: transferring the dilute acetic acid into a hydrolysis tank, starting the hydrolysis tank to stir, starting interlayer steam, and heating to 80 ℃;
1.3: dropwise adding a residue diluent, controlling the temperature of the kettle to be not too high, controlling the temperature of the kettle to be 95 ℃ after dropwise adding, and keeping full reflux in the titration reaction process;
1.4: after the dropwise addition, preserving the heat for 2 hours, and transferring the reacted hydrolysate to a transfer tank;
second, continuous separation operation of hydrolysate
2.1: starting a feeding pump, and controlling the feeding flow by adjusting the variable frequency of the feeding pump;
2.2: starting an acetone reflux pump, controlling the temperature of the tower top by controlling the acetone reflux amount, and automatically controlling the reflux amount by the temperature of the tower top;
2.3: the liquid level at the bottom of the tower is set, and the liquid level in the tower is stabilized through an electric V-shaped ball valve, so that the automatic control of the liquid level at the bottom of the tower is realized;
2.4: the steam pressure of the reboiler is set, and the steam regulating valve automatically controls the size of a steam valve according to the set pressure, so that the automatic control of the liquid level of the reboiler is realized;
2.5: setting the temperature at the bottom of the tower to be between 100 ℃, automatically adjusting the balance in the stabilizing tower, controlling the gas phase discharge through the pressure of a reboiler, setting the pressure of the reboiler, and controlling the discharge amount through the opening of a pressure control regulating valve;
2.6: the liquid level of the reboiler is set, and an electric V-shaped ball valve for controlling the discharge of the residual liquid is used for realizing the automatic adjustment of the liquid level of the reboiler.
Example 3: a method for hydrolyzing diketene residue comprises the following specific steps:
first, hydrolysis and dropping operation
1.1: transferring the distillation residues into a residue diluting tank, diluting with the liquid after pumping, and then, pressing the residue in the diluting tank into a high-level tank by using the diluted liquid;
1.2: transferring the dilute acetic acid into a hydrolysis tank, starting the hydrolysis tank to stir, starting interlayer steam, and heating to 90 ℃;
1.3: dripping residue diluent, controlling the temperature of the kettle to be not too high, controlling the temperature of the kettle to be 110 ℃ after dripping, and keeping full reflux in the titration reaction process;
1.4: after the dropwise addition, preserving the heat for 2 hours, and transferring the reacted hydrolysate to a transfer tank;
second, continuous separation operation of hydrolysate
2.1: starting a feeding pump, and controlling the feeding flow by adjusting the variable frequency of the feeding pump;
2.2: starting an acetone reflux pump, controlling the temperature of the tower top by controlling the acetone reflux amount, and automatically controlling the reflux amount by the temperature of the tower top;
2.3: the liquid level at the bottom of the tower is set, and the liquid level in the tower is stabilized through an electric V-shaped ball valve, so that the automatic control of the liquid level at the bottom of the tower is realized;
2.4: the steam pressure of the reboiler is set, and the steam regulating valve automatically controls the size of a steam valve according to the set pressure, so that the automatic control of the liquid level of the reboiler is realized;
2.5: setting the temperature at the bottom of the tower to be 110 ℃, automatically adjusting the balance in the stabilizing tower, controlling the gas phase discharge through the pressure of a reboiler, setting the pressure of the reboiler, and controlling the discharge amount through the opening of a pressure control regulating valve;
2.6: the liquid level of the reboiler is set, and an electric V-shaped ball valve for controlling the discharge of the residual liquid is used for realizing the automatic adjustment of the liquid level of the reboiler.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (4)
1. A method for hydrolyzing diketene residue is characterized by comprising the following steps:
first, hydrolysis and dropping operation
1.1: transferring the distillation residues into a residue diluting tank, diluting with the liquid after pumping, and then, pressing the residue in the diluting tank into a high-level tank by using the diluted liquid;
1.2: transferring the dilute acetic acid into a hydrolysis tank, starting the hydrolysis tank to stir, starting the interlayer steam, and heating;
1.3: dripping residue diluent, controlling the temperature of the kettle, and keeping full reflux in the titration reaction process;
1.4: after the dropwise addition, preserving the heat for 2 hours, and transferring the reacted hydrolysate to a transfer tank;
second, continuous separation operation of hydrolysate
2.1: starting a feeding pump, and controlling the feeding flow by adjusting the variable frequency of the feeding pump;
2.2: starting an acetone reflux pump, controlling the temperature of the tower top by controlling the acetone reflux amount, and automatically controlling the reflux amount by the temperature of the tower top;
2.3: the liquid level at the bottom of the tower is set, and the liquid level in the tower is stabilized through an electric V-shaped ball valve, so that the automatic control of the liquid level at the bottom of the tower is realized;
2.4: the steam pressure of the reboiler is set, and the steam regulating valve automatically controls the size of a steam valve according to the set pressure, so that the automatic control of the liquid level of the reboiler is realized;
2.5 setting the temperature at the bottom of the tower, automatically adjusting the balance in the stabilizing tower, controlling the gas phase discharge through the pressure of a reboiler, setting the pressure of the reboiler, and controlling the discharge amount through the opening of a pressure control regulating valve;
2.6: the liquid level of the reboiler is set, and an electric V-shaped ball valve for controlling the discharge of the residual liquid is used for realizing the automatic adjustment of the liquid level of the reboiler.
2. The method for hydrolysis treatment of diketene residue as claimed in claim 1, wherein in step 1.2, the heating temperature is from 70 to 90 ℃.
3. The method for hydrolysis treatment of diketene residue as claimed in claim 1, wherein in step 1.3, the temperature of the kettle is controlled to be 80-110 ℃ after the dropwise addition.
4. The method for hydrolysis treatment of diketene residue as claimed in claim 1, wherein in step 2.5, the temperature of the bottom of the column is set to be in the range of 90-110 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911381490.3A CN110981717A (en) | 2019-12-28 | 2019-12-28 | Hydrolysis treatment method for diketene residue |
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| CN201911381490.3A CN110981717A (en) | 2019-12-28 | 2019-12-28 | Hydrolysis treatment method for diketene residue |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521198A (en) * | 2022-09-16 | 2022-12-27 | 宁波王龙科技股份有限公司 | Diluted acid hydrolysis process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402670A (en) * | 2014-09-27 | 2015-03-11 | 安徽金禾实业股份有限公司 | Clean production method of diketene |
| CN105111052A (en) * | 2015-08-22 | 2015-12-02 | 安徽金禾实业股份有限公司 | Method for purifying acetone from waste residue and waste water produced in ketene dimmer production process |
-
2019
- 2019-12-28 CN CN201911381490.3A patent/CN110981717A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402670A (en) * | 2014-09-27 | 2015-03-11 | 安徽金禾实业股份有限公司 | Clean production method of diketene |
| CN105111052A (en) * | 2015-08-22 | 2015-12-02 | 安徽金禾实业股份有限公司 | Method for purifying acetone from waste residue and waste water produced in ketene dimmer production process |
Non-Patent Citations (1)
| Title |
|---|
| 申奕 等: "《化工典型设备操作技术》", 31 January 2014, 天津大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115521198A (en) * | 2022-09-16 | 2022-12-27 | 宁波王龙科技股份有限公司 | Diluted acid hydrolysis process |
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Application publication date: 20200410 |
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