CN103554079A - Method for recycling waste alkali liquor in polyformaldehyde device - Google Patents
Method for recycling waste alkali liquor in polyformaldehyde device Download PDFInfo
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- CN103554079A CN103554079A CN201310589802.6A CN201310589802A CN103554079A CN 103554079 A CN103554079 A CN 103554079A CN 201310589802 A CN201310589802 A CN 201310589802A CN 103554079 A CN103554079 A CN 103554079A
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- dioxolane
- tower
- percentage composition
- formaldehyde
- sodium hydroxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D323/00—Heterocyclic compounds containing more than two oxygen atoms as the only ring hetero atoms
- C07D323/04—Six-membered rings
- C07D323/06—Trioxane
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/12—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
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- Organic Chemistry (AREA)
- Heterocyclic Compounds That Contain Two Or More Ring Oxygen Atoms (AREA)
Abstract
The invention discloses a method for recycling waste alkali liquor in a polyformaldehyde device. The method comprises the following steps: (1) respectively delivering formaldehyde and ethanol into a dioxolane synthesizing tower; (2) delivering a gas phase material at the top of the dioxolane synthesizing tower into a dioxolane concentrating tower so as to remove ethylene glycol and the majority of formaldehyde in dioxolane; (3) cooling and delivering a gas phase discharged material at the top of the dioxolane synthesizing tower into an extraction tower, and extracting by adopting sodium hydroxide with mass percentage of greater than 45%; (4) delivering the dioxolane, with mass percentage of greater than 98%, obtained from the top of the extraction tower into a rectifying tower for purifying; and transporting the waste sodium hydroxide alkali liquor, with mass percentage of 30-35%, obtained from the bottom of the extraction tower to the polyformaldehyde device to prepare a sodium hydroxide solution with mass percentage of 10% below so as to be used for producing trioxymethylene. Any influence on the quality of trioxymethylene products can not be caused by adopting the method.
Description
Technical field
The present invention relates to a kind of recoverying and utilizing method of waste lye, the invention particularly relates to the recoverying and utilizing method of waste lye in a kind of polyoxymethylene device.
Background technology
Sodium hydroxide (concentration >=45%) has two kinds of purposes in polyoxymethylene is produced, a kind of is as the extraction agent in the production of intermediates dioxolane, with sodium hydroxide more than 45% concentration, as extraction agent, a large amount of moisture content in dioxolane are extracted, to improve the concentration of dioxolane.The sodium hydroxide that another purposes is is 45% using concentration is diluted to the following formic acid neutralizing agent in trioxymethylene is produced of 10% concentration, in order to the formic acid in removal system, to reduce the corrosion of equipment.Wherein, in the production of dioxolane, by producing a large amount of waste lyes, for sale at a low price, caused huge waste.
Summary of the invention
The object of the present invention is to provide a kind of making rational use of resources, reduce costs, do not affect the quality product of trioxymethylene and dioxolane, and can reduce the recoverying and utilizing method of waste lye in a kind of polyoxymethylene device of use of 45% sodium hydroxide and de-mineralized water.
The object of the invention is to realize by following proposal.
The recoverying and utilizing method of waste lye in a kind of polyoxymethylene device of the present invention, it comprises the following steps:
(1) formaldehyde and ethylene glycol are sent into respectively to dioxolane synthetic tower and prepare dioxolane, the reaction mol ratio of described formaldehyde and ethylene glycol is between 1.01～1.1;
(2) the top gaseous phase material of dioxolane synthetic tower is sent into dioxolane upgrading tower to remove ethylene glycol and the most of formaldehyde in dioxolane, the column bottom temperature of dioxolane upgrading tower is 98-102 ℃, trim the top of column is than being 1.5-2, and at the bottom of tower, produced quantity is 120kg/h-150kg/h;
(3) after the discharging of dioxolane upgrading tower top gaseous phase is cooling, sending into extraction tower adopts quality percentage composition to be greater than 45% oxygen sodium hydroxide solution to extract, in the discharging of dioxolane upgrading tower top gaseous phase, dioxolane quality percentage composition is 90-92%, quality of glycol percentage composition is zero, formaldehyde and methanol quality percentage composition are for being not more than 2%, and surplus is water;
(4) quality percentage composition extraction tower tower top being obtained is greater than 98% dioxolane and sends into rectifying tower and purify; Extraction tower tower substrate amount percentage composition is delivered to trioxymethylene device at the sodium hydroxide waste lye of 30-35% and is deployed into the production for trioxymethylene at the sodium hydroxide solution below 10% of quality percentage composition.
The waste lye that adopts the inventive method to produce, impurities is mainly water, also contains in addition trace formaldehyde, methyl alcohol and dioxolane etc.These impurity originally exist in the production of trioxymethylene, can gently be boiled in tower and be removed by trioxymethylene, so the quality product of trioxymethylene is not had any impact.
Accompanying drawing explanation
Accompanying drawing is the process flow sheet of the recoverying and utilizing method of waste lye in a kind of polyoxymethylene device of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is described further:
The recoverying and utilizing method of waste lye in a kind of polyoxymethylene device of the present invention as shown in drawings, it comprises the following steps: (1) is sent formaldehyde and ethylene glycol into respectively dioxolane synthetic tower and prepared dioxolane, and the reaction mol ratio of described formaldehyde and ethylene glycol is between 1.01～1.1; (2) the top gaseous phase material of dioxolane synthetic tower is sent into dioxolane upgrading tower to remove ethylene glycol and the most of formaldehyde in dioxolane, the column bottom temperature of dioxolane upgrading tower is 98-102 ℃, trim the top of column is than being 1.5-2, and at the bottom of tower, produced quantity is 120kg/h-150kg/h; (3) after the discharging of dioxolane upgrading tower top gaseous phase is cooling, sending into extraction tower adopts quality percentage composition to be greater than 45% oxygen sodium hydroxide solution to extract, in the discharging of dioxolane upgrading tower top gaseous phase, dioxolane quality percentage composition is 90-92%, quality of glycol percentage composition is zero, formaldehyde and methanol quality percentage composition are for being not more than 2%, and surplus is water; At the bottom of dioxolane upgrading tower tower, discharging goes recovery tower to recycle; (4) quality percentage composition extraction tower tower top being obtained is greater than 98% dioxolane and sends into rectifying tower and purify; Extraction tower tower substrate amount percentage composition is delivered to trioxymethylene device at the sodium hydroxide waste lye of 30-35% and is deployed into the production for trioxymethylene at the sodium hydroxide solution below 10% of quality percentage composition.
Embodiment 1
(1) formaldehyde and ethylene glycol are sent into respectively to dioxolane synthetic tower and prepare dioxolane, the reaction mol ratio of described formaldehyde and ethylene glycol is 1.01; (2) the top gaseous phase material of dioxolane synthetic tower is sent into dioxolane upgrading tower to remove ethylene glycol and the most of formaldehyde in dioxolane, the column bottom temperature of dioxolane upgrading tower is 102 ℃, and trim the top of column ratio is 2, and at the bottom of tower, produced quantity is 150kg/h; (3) after the discharging of dioxolane upgrading tower top gaseous phase is cooling, sending into extraction tower adopts quality percentage composition to be greater than 45% oxygen sodium hydroxide solution to extract; In the discharging of dioxolane upgrading tower top gaseous phase, dioxolane quality percentage composition is 91%, and quality of glycol percentage composition is zero, and formaldehyde and methanol quality percentage composition are for being not more than 2%, and surplus is water; (4) quality percentage composition extraction tower tower top being obtained is greater than 98% dioxolane and sends into rectifying tower and purify; Sodium hydroxide waste lye at the bottom of extraction tower tower is delivered to trioxymethylene device and is deployed into the production for trioxymethylene at the sodium hydroxide solution below 10% of quality percentage composition.
By the present invention, resulting waste lye quality group becomes: sodium hydroxide 30.8%, and water 68.0%, formaldehyde 1%, methyl alcohol 0.2%, ethylene glycol does not detect, and meets trioxymethylene production requirement completely.
Embodiment 2
(1) formaldehyde and ethylene glycol are sent into respectively to dioxolane synthetic tower and prepare dioxolane, the reaction mol ratio of described formaldehyde and ethylene glycol is 1.1; (2) the top gaseous phase material of dioxolane synthetic tower is sent into dioxolane upgrading tower to remove ethylene glycol and the most of formaldehyde in dioxolane, the column bottom temperature of dioxolane upgrading tower is 98 ℃, and trim the top of column ratio is 1.5, and at the bottom of tower, produced quantity is 120kg/h; (3) after the discharging of dioxolane upgrading tower top gaseous phase is cooling, sending into extraction tower adopts quality percentage composition to be greater than 45% oxygen sodium hydroxide solution to extract; In the discharging of dioxolane upgrading tower top gaseous phase, dioxolane quality percentage composition is 90%, and quality of glycol percentage composition is zero, and formaldehyde and methanol quality percentage composition are for being not more than 2%, and surplus is water; (4) quality percentage composition extraction tower tower top being obtained is greater than 98% dioxolane and sends into rectifying tower and purify; Sodium hydroxide waste lye at the bottom of extraction tower tower is delivered to trioxymethylene device and is deployed into the production for trioxymethylene at the sodium hydroxide solution below 10% of quality percentage composition.
By the present invention, resulting waste lye quality group becomes: sodium hydroxide 31.3%, and water 66.7.%, formaldehyde 1.9%, methyl alcohol 0.1%, ethylene glycol does not detect, and meets trioxymethylene production requirement completely.
Embodiment 3
(1) formaldehyde and ethylene glycol are sent into respectively to dioxolane synthetic tower and prepare dioxolane, the reaction mol ratio of described formaldehyde and ethylene glycol is 1.05; (2) the top gaseous phase material of dioxolane synthetic tower is sent into dioxolane upgrading tower to remove ethylene glycol and the most of formaldehyde in dioxolane, the column bottom temperature of dioxolane upgrading tower is 100 ℃, trim the top of column ratio is 1.8, and at the bottom of tower, produced quantity is 130kg/h; (3) after the discharging of dioxolane upgrading tower top gaseous phase is cooling, sending into extraction tower adopts quality percentage composition to be greater than 45% oxygen sodium hydroxide solution to extract; In the discharging of dioxolane upgrading tower top gaseous phase, dioxolane quality percentage composition is 92%, and quality of glycol percentage composition is zero, and formaldehyde and methanol quality percentage composition are for being not more than 2%, and surplus is water; (4) quality percentage composition extraction tower tower top being obtained is greater than 98% dioxolane and sends into rectifying tower and purify; Sodium hydroxide waste lye at the bottom of extraction tower tower is delivered to trioxymethylene device and is deployed into the production for trioxymethylene at the sodium hydroxide solution below 10% of quality percentage composition.
By the present invention, resulting waste lye quality group becomes: sodium hydroxide 34.8%, and water 63.5%, formaldehyde 1.5%, methyl alcohol 0.2%, ethylene glycol does not detect, and meets trioxymethylene production requirement completely.
Claims (1)
1. a recoverying and utilizing method for waste lye in polyoxymethylene device, is characterized in that it comprises the following steps:
(1) formaldehyde and ethylene glycol are sent into respectively to dioxolane synthetic tower and prepare dioxolane, the reaction mol ratio of described formaldehyde and ethylene glycol is between 1.01～1.1;
(2) the top gaseous phase material of dioxolane synthetic tower is sent into dioxolane upgrading tower to remove ethylene glycol and the most of formaldehyde in dioxolane, the column bottom temperature of dioxolane upgrading tower is 98-102 ℃, trim the top of column is than being 1.5-2, and at the bottom of tower, produced quantity is 120kg/h-150kg/h;
(3) after the discharging of dioxolane upgrading tower top gaseous phase is cooling, sending into extraction tower adopts quality percentage composition to be greater than 45% oxygen sodium hydroxide solution to extract, in the discharging of dioxolane upgrading tower top gaseous phase, dioxolane quality percentage composition is 90-92%, quality of glycol percentage composition is zero, formaldehyde and methanol quality percentage composition are for being not more than 2%, and surplus is water;
(4) quality percentage composition extraction tower tower top being obtained is greater than 98% dioxolane and sends into rectifying tower and purify; Extraction tower tower substrate amount percentage composition is delivered to trioxymethylene device at the sodium hydroxide waste lye of 30-35% and is deployed into the production for trioxymethylene at the sodium hydroxide solution below 10% of quality percentage composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310589802.6A CN103554079A (en) | 2013-11-20 | 2013-11-20 | Method for recycling waste alkali liquor in polyformaldehyde device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310589802.6A CN103554079A (en) | 2013-11-20 | 2013-11-20 | Method for recycling waste alkali liquor in polyformaldehyde device |
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| CN103554079A true CN103554079A (en) | 2014-02-05 |
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| CN201310589802.6A Pending CN103554079A (en) | 2013-11-20 | 2013-11-20 | Method for recycling waste alkali liquor in polyformaldehyde device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108516968A (en) * | 2018-05-03 | 2018-09-11 | 开封龙宇化工有限公司 | It is a kind of recycling dioxolane reboiling tower bottom material device and technological process |
| US10585514B2 (en) | 2017-05-22 | 2020-03-10 | Boe Technology Group Co., Ltd. | Pixel circuit, display panel and driving method thereof |
| CN111848889A (en) * | 2020-08-14 | 2020-10-30 | 中化学科学技术研究有限公司 | Method for preparing polyformaldehyde by coproduction of trioxymethylene and dioxolane |
-
2013
- 2013-11-20 CN CN201310589802.6A patent/CN103554079A/en active Pending
Non-Patent Citations (3)
| Title |
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| "萃取工艺在三聚甲醛生产应用中的优化": ""萃取工艺在三聚甲醛生产应用中的优化"", 《煤化工》 * |
| 刘继泉等: ""反应萃取精馏技术生产二氧五环的工艺研究"", 《青岛科技大学学报(自然科学版)》 * |
| 邵淇渝等: ""浅谈二氧五环工艺生产过程及物质特性", 《科技传播》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10585514B2 (en) | 2017-05-22 | 2020-03-10 | Boe Technology Group Co., Ltd. | Pixel circuit, display panel and driving method thereof |
| CN108516968A (en) * | 2018-05-03 | 2018-09-11 | 开封龙宇化工有限公司 | It is a kind of recycling dioxolane reboiling tower bottom material device and technological process |
| CN111848889A (en) * | 2020-08-14 | 2020-10-30 | 中化学科学技术研究有限公司 | Method for preparing polyformaldehyde by coproduction of trioxymethylene and dioxolane |
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Application publication date: 20140205 |