CN103708996A - Method for recycling methanol with rectification tower - Google Patents

Method for recycling methanol with rectification tower Download PDF

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Publication number
CN103708996A
CN103708996A CN201310692581.5A CN201310692581A CN103708996A CN 103708996 A CN103708996 A CN 103708996A CN 201310692581 A CN201310692581 A CN 201310692581A CN 103708996 A CN103708996 A CN 103708996A
Authority
CN
China
Prior art keywords
tower
low levels
aqueous solution
methyl alcohol
methanol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201310692581.5A
Other languages
Chinese (zh)
Inventor
周灿方
裴增昌
顾红军
张剑飞
高瞻
余俊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
DSM Jiangshan Pharmaceutical Jiangsu Co Ltd
Original Assignee
Aland Jiangsu Nutraceutical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Aland Jiangsu Nutraceutical Co Ltd filed Critical Aland Jiangsu Nutraceutical Co Ltd
Priority to CN201310692581.5A priority Critical patent/CN103708996A/en
Publication of CN103708996A publication Critical patent/CN103708996A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation

Abstract

The invention discloses a method for recycling methanol with a rectification tower, which comprises the following steps: 1. rectifying a low-content methanol water solution through a rectification tower; 2. preheating the low-content methanol water solution to 50-60 DEG C by fully utilizing the steam exhaust in the product production process, and sending the low-content methanol water solution into the rectification tower to perform recycling; and 3. controlling the pressure of the pressurization tower by continuous pressure relief to send small amount of unqualified methanol methanol into the atmospheric tower so as to continue recycling, thereby implementing the stable operation of the rectification tower. The method enhances the recovery rate of methanol, lowers the production cost and reduces the environmental pollution.

Description

Utilize rectifying tower to reclaim the method for methyl alcohol
Technical field
The present invention relates to a kind of method that reclaims methyl alcohol, particularly relate to a kind of method of utilizing rectifying tower to reclaim methyl alcohol.
Background technology
In vitamin C producing process, methyl alcohol is as organic solvent, in ascorbic each production phase, participate in the unit operations such as chemical reaction, crystallisation process, usage quantity is large, the low levels methyl alcohol occurring in production process, can not efficient recovery, directly be disposed to environmental protection treatment, methyl alcohol waste is large, has increased environmental protection treatment cost simultaneously.The work such as energy-saving and cost-reducing, environmental improvement are the existence problems that production of vitamin C enterprise faces always.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of utilizing rectifying tower to reclaim methyl alcohol, and it improves Methanol Recovery rate, reduces production costs, and reduces environmental pollution.
The present invention solves above-mentioned technical problem by following technical proposals: a kind of method of utilizing rectifying tower to reclaim methyl alcohol, it is characterized in that, and it comprises the following steps:
Step 1, carries out rectifying by low levels methanol aqueous solution by rectifying tower;
Step 2, makes full use of the steam tail gas in process of producing product, and then temperature to 50 ~ 60 ℃ of preheating low levels methanol aqueous solution enter rectifying tower and reclaim;
Step 3, controls pressurizing tower pressure by lasting pressure release, and a small amount of defective methyl alcohol is entered to the steady running that atmospheric tower continues to retrieve to realize rectifying tower.
Preferably, the reflux ratio of described process control tower is 6:1, and top temperature is 75 ℃ ~ 80 ℃.
Preferably, the intake of described low levels methanol aqueous solution amount is 25 ~ 30m 3/ h, the heating steam flow of process control tower is 7 ~ 7.5t/h.
Preferably, after the preheating of described low levels methanol aqueous solution, form the solidifying water of low levels methanol aqueous solution.
Positive progressive effect of the present invention is: the present invention utilizes double-effect rectification tower to reclaim methyl alcohol to the solidifying water of the low levels methyl alcohol producing in vitamin C producing process, the present invention is by being preheating to after certain temperature by the solidifying aqueous solution of low levels methyl alcohol, enter methanol rectifying tower, by controlling the measures such as reflux ratio and pressurizing tower pressure, guaranteeing on the basis of rectifying tower steady running, obtain the recovery methyl alcohol of high-content, reduce the methanol consumption in production of vitamin C, save production cost.The present invention has overcome normal productive process methanol rectifying tower to entering the requirement of tower methanol content, has improved the adaptability of methanol column.
Embodiment
The method that the present invention utilizes rectifying tower to reclaim methyl alcohol comprises the following steps:
Step 1, carries out rectifying by low levels methanol aqueous solution by rectifying tower; The intake of described low levels methanol aqueous solution amount is 25 ~ 30m 3/ h, the heating steam flow of process control tower is 7 ~ 7.5t/h.
Step 2, makes full use of the steam tail gas in process of producing product, and then temperature to 50 ~ 60 ℃ of preheating low levels methanol aqueous solution enter rectifying tower and reclaim; The reflux ratio of described process control tower is 6:1, and top temperature is 75 ℃ ~ 80 ℃.After the preheating of low levels methanol aqueous solution, form the solidifying water of low levels methanol aqueous solution.
Step 3, controls pressurizing tower pressure by lasting pressure release, and a small amount of defective methyl alcohol is entered to the steady running that atmospheric tower continues to retrieve to realize rectifying tower.
A concrete test example of the present invention is as follows: the low levels methanol aqueous solution 250m in centralized collection production process 3and carry out rectifying, and making full use of the steam tail gas in process of producing product, temperature to 50 ~ 60 ℃ of preheating low levels methanol aqueous solution, with 25 m 3the flow of/h enters methanol column and carries out rectifying recovery, and the heating steam flow of process control tower is 7.5 t/h, and reflux ratio is 6:1, and tower top temperature (being called for short " top temperature ") is 76 ℃ ~ 80 ℃, and continuous production 10 hours, by metering, obtains 90% 21 m 3high carbinol content, steam usage quantity is 72.6T.
Another concrete test example of the present invention is as follows: the low levels methanol aqueous solution 200m in centralized collection production process 3and carry out rectifying, and making full use of the steam tail gas in process of producing product, temperature to 50 ~ 60 ℃ of preheating low levels methanol aqueous solution, with 30 m 3the flow of/h enters methanol column and carries out rectifying recovery, and the heating steam flow of process control tower is 7.0 t/h, and reflux ratio is 6:1, and tower top temperature is 75 ℃ ~ 77 ℃, and continuous production 8 hours, by metering, obtains 93% 16.5 m 3high carbinol content, steam usage quantity is 56T.
The present invention makes full use of the steam tail gas in vitamin C producing process, temperature to 50 ~ 60 ℃ of preheating low levels methanol aqueous solution, then enter rectifying tower and reclaim, can effectively reduce the consumption to steam in low levels methanol aqueous solution removal process, save cost recovery.Pressurizing tower hypertonia while operating due to low levels Methanol Recovery, the pressure tolerance band that exceeds tower, process is controlled pressurizing tower pressure by lasting pressure release, and continue to go out defective methyl alcohol to atmospheric tower, when providing thermal source to atmospheric tower, a small amount of defective methyl alcohol is entered to atmospheric tower and continue to reclaim, realize the steady running of tower.The reflux ratio 6:1 of process control tower of the present invention, 75 ℃ ~ 80 ℃ of top temperature, the high carbinol content solution of acquisition 90% left and right, can be used for producing, and has improved Methanol Recovery rate.The present invention reclaims by the tower that enters of the solidifying water of low levels methanol aqueous solution, has played the effect of cleaning reboiler, has solved the easy carbon deposit of rectifying tower removal process reboiler and has stopped up a difficult problem; In waste water, methyl alcohol is realized zero release substantially, has reduced environmental influence.
The invention is not restricted to these disclosed embodiment; the present invention is by the described scope of soverlay technique scheme; and the various distortion of claim scope and equivalence variation; do not departing under the prerequisite of technical solution of the present invention, any modification that those skilled in the art made for the present invention easily realize or improvement all belong to the present invention's scope required for protection.

Claims (4)

1. utilize rectifying tower to reclaim a method for methyl alcohol, it is characterized in that, it comprises the following steps:
Step 1, carries out rectifying by low levels methanol aqueous solution by rectifying tower;
Step 2, makes full use of the steam tail gas in process of producing product, and then temperature to 50 ~ 60 ℃ of preheating low levels methanol aqueous solution enter rectifying tower and reclaim;
Step 3, controls pressurizing tower pressure by lasting pressure release, and a small amount of defective methyl alcohol is entered to the steady running that atmospheric tower continues to retrieve to realize rectifying tower.
2. the method for utilizing rectifying tower to reclaim methyl alcohol as claimed in claim 1, is characterized in that, the reflux ratio of described process control tower is 6:1, and top temperature is 75 ℃ ~ 80 ℃.
3. the method for utilizing rectifying tower to reclaim methyl alcohol as claimed in claim 1, is characterized in that, the intake of described low levels methanol aqueous solution amount is 25 ~ 30m 3/ h, the heating steam flow of process control tower is 7 ~ 7.5t/h.
4. the method for utilizing rectifying tower to reclaim methyl alcohol as claimed in claim 1, is characterized in that, forms the solidifying water of low levels methanol aqueous solution after the preheating of described low levels methanol aqueous solution.
CN201310692581.5A 2013-12-18 2013-12-18 Method for recycling methanol with rectification tower Pending CN103708996A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310692581.5A CN103708996A (en) 2013-12-18 2013-12-18 Method for recycling methanol with rectification tower

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310692581.5A CN103708996A (en) 2013-12-18 2013-12-18 Method for recycling methanol with rectification tower

Publications (1)

Publication Number Publication Date
CN103708996A true CN103708996A (en) 2014-04-09

Family

ID=50402389

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310692581.5A Pending CN103708996A (en) 2013-12-18 2013-12-18 Method for recycling methanol with rectification tower

Country Status (1)

Country Link
CN (1) CN103708996A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981034A (en) * 2014-05-19 2014-08-13 东莞新宝精化有限公司 Method and special device for continuously recycling methanol tail gas in biodiesel production
CN106220473A (en) * 2016-08-29 2016-12-14 查都(上海)科技有限公司 A kind of wastewater of rectification recovery system

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760164A (en) * 2005-10-27 2006-04-19 天津大学 Energy saving equipment of double effect rectification for methanol, and method
CN101190874A (en) * 2007-12-21 2008-06-04 天津大学 Magnetization rectification method for reclaiming methanol from waste methanol menstruum

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1760164A (en) * 2005-10-27 2006-04-19 天津大学 Energy saving equipment of double effect rectification for methanol, and method
CN101190874A (en) * 2007-12-21 2008-06-04 天津大学 Magnetization rectification method for reclaiming methanol from waste methanol menstruum

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103981034A (en) * 2014-05-19 2014-08-13 东莞新宝精化有限公司 Method and special device for continuously recycling methanol tail gas in biodiesel production
CN106220473A (en) * 2016-08-29 2016-12-14 查都(上海)科技有限公司 A kind of wastewater of rectification recovery system

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Application publication date: 20140409