CN109622535A - A kind of method of rapid cleaning rectifying column - Google Patents
A kind of method of rapid cleaning rectifying column Download PDFInfo
- Publication number
- CN109622535A CN109622535A CN201811638911.1A CN201811638911A CN109622535A CN 109622535 A CN109622535 A CN 109622535A CN 201811638911 A CN201811638911 A CN 201811638911A CN 109622535 A CN109622535 A CN 109622535A
- Authority
- CN
- China
- Prior art keywords
- tower
- cleaning
- rectifying
- tower reactor
- reflux
- 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
Links
- 238000004140 cleaning Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- 239000013557 residual solvent Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 11
- 238000005406 washing Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229930186147 Cephalosporin Natural products 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229940124587 cephalosporin Drugs 0.000 description 1
- 150000001780 cephalosporins Chemical class 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003640 drug residue Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
- B08B9/093—Cleaning containers, e.g. tanks by the force of jets or sprays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
The invention belongs to cleaning equipment fields, and in particular to a kind of method of rapid cleaning rectifying column.This method includes washing, alkali cleaning, washes again.The present invention optimizes improvement on the basis of original cleaning, using rectification under vacuum ablution compared with conventional atmospheric rectifying ablution, not only can be shortened the cleaning frequency, and solvent residual and activity substance content are lower in tower.
Description
Technical field
The invention belongs to cleaning equipment fields, and in particular to a kind of method of rapid cleaning rectifying device.
Background technique
In medication chemistry or fine chemistry industry, multiple kinds are usually produced, change in kind rectifying production, is needing to essence
It evaporates tower thoroughly to be cleaned, if the cleaning frequency is short, it may not be possible to which cleaning thoroughly, can cause the production of next kind to intersect dirty
Dye；If the cleaning frequency is longer, can thorough cleaning equipment, but the cleaning frequency it is longer be unfavorable for producing, cause the entire production cycle
Extension, be unfavorable for producing.Therefore need to find a kind of method of rapid cleaning rectifying device.Due to testing kind in laboratory
It is more, it needs often to switch kind and carries out rectifying experiment, the frequency for cleaning tower is relatively high, not only needs when cleaning tower by solvent
Residual cleaning is thoroughly, still critically important to medicament residue cleaning requirement, and the shorter the cleaning qualified required cleaning frequency the better.
For rectifying column when changing variety production, about the pertinent literature and patent for cleaning rectifying column, there is not been reported, the present invention
A kind of method of rapid cleaning rectifying column is provided, this method can also promote amplification, and cleaning effect is obvious, and the period is shorter.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of methods of rapid cleaning rectifying device, and cleaning equipment is not only
Solvent residual is less, and medicament residue is also qualified, and the entire cleaning frequency is shorter compared with the conventional cleaning device period.
Technical solution provided by the invention is as follows:
(1) it checks: first checking for material inlet valve, it is ensured that valve belongs to open state；
(2) first pass cleans, and washing: being continuously added to rectifying column, flush feed pipeline and rectifying column for water by feed pump,
Waste liquid produces pump discharge by tower reactor；It pumps again by extracted feed to tower reactor and water is added, heating mantle heats switch is opened, to tower
Kettle heating, opens vacuum system, and extraction product is arranged back in receiving tank after keeping tower pressure interior force, condensation tower head to generate reflux
Stream ratio is to detect organic phase content in phegma using Agilent gas chromatograph external standard method after 1,0.5 hour, when detection solvent
When residual quantity is less than 500mg/L, tower is washed in stopping, and kettle is residual in discharge tower reactor and receives pot liquid to wastewater barrel；
(3) second times cleanings, alkali cleaning: configuring certain density sodium hydroxide solution, is pumped by extracted feed and adds lye
Enter in rectifying column, opens heating mantle heats switch, open vacuum system, keep tower pressure interior force, reflux ratio is set as 1, rectifying 0.5
After hour, flow liquid detection medicament residue is fetched, when activity substance content cannot be detected, tower is washed in stopping, and discharge kettle is residual and returns
Pot liquid is flowed into waste liquid barrel；
(4) third is washed again all over cleaning: by extracted feed pump rectifying tower reactor is added in water again, is opened heating mantle
Heater switch heats tower reactor, opens vacuum system, keeps tower pressure interior force, starts to produce after generating reflux, after producing 0.5h,
Distillate pH value is detected, after overhead distillate and tower reactor Produced Liquid pH are 7.0-8.0, tower is washed in stopping, and discharge kettle is residual and return tank
Interior liquid is to wastewater barrel.
Preferably, the tower pressure interior force is 20-30KPa.
Preferably, the sodium hydroxide molar concentration is 1%.
The invention has the advantages that can thoroughly clean solvent residual and medicament residue, peace in tower using three times rectification under vacuum ablutions
Prompt human relations vapor detection result can be tracked to tower situation is washed, it is ensured that solvent residual and drug residue are qualified in tower, and product is clear
It is short compared with the conventional atmospheric rectifying cleaning frequency to wash the period.
Detailed description of the invention
Attached drawing 1 is the process flow chart of rapid cleaning rectifying column.
In figure: 01- feed pump 02- extractant feed pumps 03,04,10,11,13- valve 05- intelligent temperature control electric heating
It covers 06- tower reactor 07- rectifying column 08- condensation tower head 09- product and produces receiving tank 12-U type vacuum meter 14- vacuum buffer tank
16 tower reactor of the 15- vacuum pump extraction pump residual receiving tank of 17- kettle
Specific embodiment
Summary of the invention of the invention is described in further detail below by specific embodiment, but is not therefore limited
Determine the contents of the present invention.
The invention mainly relates to a kind of methods of rapid cleaning rectifying column, carry out rectifying to cephalo-type medicine solvent mother liquor 1
After change before another kind of cephalosporins medicine solvent mother liquor 2 carries out rectifying, need thoroughly to be washed tower, the specific steps are as follows:
(1) it checks: first checking for material inlet valve, it is ensured that valve belongs to open state；
(2) first pass cleans, and washing: water is continuously added to rectifying column by feed pump, inlet amount 2L is flushed into expects pipe
Line and rectifying column, waste liquid produce pump discharge by tower reactor.It pumps again by extracted feed to tower reactor and 3L water is added, open heating mantle
Heater switch heats tower reactor, opens vacuum system, starts after keeping tower pressure interior force 20-30KPa, condensation tower head to generate reflux
Product is produced in receiving tank, reflux ratio is flowed back after being set as 1,0.5 hour using the detection of Agilent gas chromatograph external standard method
Organic phase content in liquid, it is qualified when solvent residual is less than 500mg/L, otherwise continue to produce, until detection Determination of Residual Solvents is small
When 0.5%, tower is washed in stopping.Kettle is residual in discharge tower reactor and receives pot liquid to wastewater barrel；
(3) second times cleanings, alkali cleaning: the sodium hydroxide solution 3L that configuration concentration is 1% is pumped by extracted feed by lye
It is added in rectifying column, opens heating mantle heats switch, open vacuum system, keep tower pressure interior force 20-30KPa, reflux ratio setting
It is 1, after rectifying 0.5 hour, fetches flow liquid detection medicament residue, when activity substance content cannot be detected, tower is washed in stopping.Row
Put kettle it is residual and reflux pot liquid into waste liquid barrel；
(4) third is washed again all over cleaning: by extracted feed pump rectifying tower reactor is added in 3L water again, is opened heating
Heater switch is covered, tower reactor is heated, opens vacuum system, opens 10,11,13 valves and vacuum pump, keeps tower pressure interior force 20-
30KPa starts to produce after generating reflux, after producing 0.5h, detects distillate pH value, overhead distillate and tower reactor Produced Liquid pH are
After 7.0-8.0, tower is washed in stopping, and discharge kettle is residual and reflux pot liquid is to wastewater barrel.
Embodiment 1-5 is to be the method using above-described embodiment for commonly using the cleaning of cephalo veriety solvent in table 1.It is right
Ratio 1-5 be by the embodiment of the present invention three times cleaning in vacuum system be changed to normal pressure system, connect with outside air progress
Cleaning, specific comparing result are shown in Table 1.
Table 1: rectifying column cleans testing result
As known from Table 1, it tower is washed using rectification under vacuum washes tower on the cleaning frequency compared with conventional atmospheric rectifying and greatly shorten；Detection
Solvent residual and activity substance content it is lower, experiment effect is far superior to normal pressure cleaning method.
It is pointed out that the technical concepts and features of above-described embodiment only to illustrate the invention, it is ripe its object is to allow
The personage for knowing technique cans understand the content of the present invention and implement it accordingly, and protection model of the invention can not be limited with this
It encloses.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of method of rapid cleaning rectifying device, which is characterized in that clean method the following steps are included:
(1) it checks: first checking for material inlet valve, it is ensured that valve belongs to open state；
(2) it washes: water being continuously added to by rectifying column by feed pump, flush feed pipeline and rectifying column, waste liquid are adopted by tower reactor
Pump discharge out；It pumps again by extracted feed to tower reactor and water is added, open heating mantle heats switch, tower reactor is heated, open true
Empty set system, extraction product is in receiving tank after keeping tower pressure interior force, condensation tower head to generate reflux, and setting reflux ratio is 1, and 0.5 is small
When after using Agilent gas chromatograph external standard method detection phegma in organic phase content, when detection Determination of Residual Solvents be less than
When 500mg/L, tower is washed in stopping, and kettle is residual in discharge tower reactor and receives pot liquid to wastewater barrel；
(3) alkali cleaning: configuring certain density sodium hydroxide solution, and lye is added in rectifying column by extracted feed pump, is opened
Heating mantle heats switch, opens vacuum system, and tower pressure interior force is kept to fetch flow liquid after reflux ratio is set as 1, rectifying 0.5 hour
Medicament residue is detected, when activity substance content cannot be detected, tower is washed in stopping, and discharge kettle is residual and reflux pot liquid is to waste liquid
In bucket；
(4) it washes again: water being added by rectifying tower reactor by extracted feed pump again, heating mantle heats switch is opened, to tower reactor
Vacuum system is opened in heating, keeps tower pressure interior force, starts to produce after generating reflux, after producing 0.5h, detects distillate pH value,
After overhead distillate and tower reactor Produced Liquid pH are 7.0-8.0, tower is washed in stopping, and discharge kettle is residual and reflux pot liquid is to wastewater barrel.
2. the method according to claim 1, wherein the tower pressure interior force is 20-30KPa.
3. the method according to claim 1, wherein the sodium hydroxide molar concentration is 1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811638911.1A CN109622535A (en) | 2018-12-29 | 2018-12-29 | A kind of method of rapid cleaning rectifying column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811638911.1A CN109622535A (en) | 2018-12-29 | 2018-12-29 | A kind of method of rapid cleaning rectifying column |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109622535A true CN109622535A (en) | 2019-04-16 |
Family
ID=66055110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811638911.1A Pending CN109622535A (en) | 2018-12-29 | 2018-12-29 | A kind of method of rapid cleaning rectifying column |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109622535A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113634003A (en) * | 2021-07-19 | 2021-11-12 | 山东明泉新材料科技有限公司 | Efficient hot washing method of methanol rectification system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273578A (en) * | 1997-10-22 | 2000-11-15 | 巴斯福股份公司 | Method for cleaning system components |
| CN105214342A (en) * | 2015-11-12 | 2016-01-06 | 河北智同生物制药有限公司 | A kind of corrosion resistant multi-functional adsorption tower and application thereof |
| CN105363237A (en) * | 2015-11-27 | 2016-03-02 | 北京首钢朗泽新能源科技有限公司 | Clean-in-place system for distillation device, preparation for cleaning liquid, and cleaning method |
| CN107243241A (en) * | 2017-05-22 | 2017-10-13 | 天伟化工有限公司 | The key of caustic wash tower one washes the control method of tower in vinyl chloride production |
-
2018
- 2018-12-29 CN CN201811638911.1A patent/CN109622535A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273578A (en) * | 1997-10-22 | 2000-11-15 | 巴斯福股份公司 | Method for cleaning system components |
| CN105214342A (en) * | 2015-11-12 | 2016-01-06 | 河北智同生物制药有限公司 | A kind of corrosion resistant multi-functional adsorption tower and application thereof |
| CN105363237A (en) * | 2015-11-27 | 2016-03-02 | 北京首钢朗泽新能源科技有限公司 | Clean-in-place system for distillation device, preparation for cleaning liquid, and cleaning method |
| CN107243241A (en) * | 2017-05-22 | 2017-10-13 | 天伟化工有限公司 | The key of caustic wash tower one washes the control method of tower in vinyl chloride production |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113634003A (en) * | 2021-07-19 | 2021-11-12 | 山东明泉新材料科技有限公司 | Efficient hot washing method of methanol rectification system |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190416 |
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| RJ01 | Rejection of invention patent application after publication |