CN106316794B - The recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution - Google Patents
The recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution Download PDFInfo
- Publication number
- CN106316794B CN106316794B CN201610694184.5A CN201610694184A CN106316794B CN 106316794 B CN106316794 B CN 106316794B CN 201610694184 A CN201610694184 A CN 201610694184A CN 106316794 B CN106316794 B CN 106316794B
- Authority
- CN
- China
- Prior art keywords
- tower
- ethyl alcohol
- temperature
- mother solution
- crystalline mother
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to chemical production technology fields, disclose the recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution, aureomycin crystalline mother solution is subjected to neutralization pretreatment, is then filtered with sheet frame, is re-fed into destilling tower after film filters, through steam heating recovery ethyl alcohol, vapo(u)rizing temperature is controlled at 70-110 DEG C, and carry out tower bottom, in tower, three temperature controls of tower top, condenser temperature controls at 50 DEG C or less, disposing mother liquor rate 50-70% is realized, the ethanol content 90-95% being recovered to.The characteristics of present invention has simple process, and the rate of recovery is high, and production cost is effectively reduced, reduces ethanol emission amount, reduces environmental pollution.
Description
Technical field
The present invention relates to the recovery methods of ethyl alcohol in chemical production technology field, especially aureomycin hydrochloride crystalline mother solution.
Background technique
Ethyl alcohol is a kind of excellent organic solvent, can dissolve many inorganic matters and many organic matters of dissolution, answer extensively
For all trades and professions.In recent years, with the fast development of animal husbandry, aureomycin hydrochloride market also constantly expands.Aureomycin hydrochloride
First aureomycin calcium and magnesium double salt is made in ferment filtrate by preparation workshop section, is added the dissolution of acidic alcohol mixed liquor, is carried out coarse crystallization, so
Coarse crystallization is dissolved in magnesium chloride ethanol solution afterwards, finally carries out being recrystallized to give aureomycin hydrochloride finished product.It is mould in hydrochloric acid gold
In element preparation production, coarse crystallization and re-crystallization stage make solvent with a large amount of ethyl alcohol.It is generated after the two stage crystallizations big
The crystalline mother solution of amount, crystalline mother solution are largely ethyl alcohol, and rest part is water, remaining aureomycin and other impurities etc..If
Ethyl alcohol is not recycled, it can not recycling.It causes ethyl alcohol to lose if direct emission, increases cost, more crucial is dirty
Contaminate environment, it is therefore necessary to recycle to the ethyl alcohol in crystalline mother solution.
Summary of the invention
The purpose of the present invention is to provide the recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution, this law simple process,
The characteristics of rate of recovery is high, and production cost is effectively reduced, reduces ethanol emission amount, reduces environmental pollution.
To realize above-mentioned technical purpose and the technique effect, the invention discloses in aureomycin hydrochloride crystalline mother solution
The recovery method of ethyl alcohol, comprises the steps that
Step 1: aureomycin hydrochloride crystalline mother solution carries out neutralization pretreatment, forms suspension, continues stirring 10-30 minutes；
Step 2: the suspension that step 1 is obtained carries out plate-frame filtering, sheet frame pressure≤0.3MPa, the filtrate warp of collection
Ethanol distillation tower is entered back into after film filtering；
Step 3: ethyl alcohol is heated by steam, vapo(u)rizing temperature is controlled at 70-110 DEG C, and carry out tower bottom, in tower, tower top three
The control of a temperature, treated that alcohol gas condenses through condenser collects subsequently into collecting tank for distillation, and wherein condenser condenses
Temperature is controlled at 50 DEG C or less.
Wherein, step 1 neutralization pretreatment is that 0.5-5%(W/V is added) calcium salt or 0-6%(W/V) magnesium salts, 10-30 points of stirring
Clock, with alkaline solution tune pH to 5.5-8.0.
Wherein, film is filtered into using ceramic membrane filter in step 2, controls inlet pressure≤0.3MPa of film, the outlet of film
Pressure 0.15-0.25MPa.
Wherein, tower bottom in step 3, in tower, three temperature controls of tower top be respectively 100-110 DEG C of column bottom temperature, tower medium temperature
80-95 DEG C, 70-80 DEG C of tower top temperature of degree.
Wherein, calcium salt be one or more of calcium carbonate, calcium sulfate, calcium nitrate, calcium phosphate, calcium oxide, calcium hydroxide,
Magnesium salts is one or more of magnesium chloride, magnesium sulfate, magnesia, and alkaline solution is ammonium hydroxide, liquid alkaline, one in 20% sodium carbonate
Kind is several.
Preferably, calcium salt is calcium carbonate, and magnesium salts is magnesium chloride, and alkaline solution is liquid alkaline.
The invention has the following advantages:
Then the present invention is filtered with sheet frame, is filtered through film by the way that aureomycin crystalline mother solution is carried out neutralization pretreatment
After be re-fed into destilling tower, through steam heating recovery ethyl alcohol, vapo(u)rizing temperature is controlled at 70-110 DEG C, and carry out tower bottom, in tower, tower
Three temperature controls are pushed up, at 50 DEG C hereinafter, realizing disposing mother liquor rate 50-70%, the ethyl alcohol being recovered to contains for condenser temperature control
Measure 90-95%.The present invention has simple process, and the rate of recovery is high, and production cost is effectively reduced, and reduces ethanol emission amount, reduces to ring
The characteristics of border is polluted.
Detailed description of the invention
Fig. 1 is flow diagram of the invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.
Embodiment 1
As shown in Figure 1, including following step the invention discloses the recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution
It is rapid:
Step 1: 0.5-5%(W/V is added in aureomycin hydrochloride crystalline mother solution) calcium salt or 0-6%(W/V) magnesium salts, stirs 10-
30 minutes, with alkaline solution tune pH to 5.5-8.0, suspension is formed, continues stirring 10-30 minutes；
Step 2: the suspension that step 1 is obtained carries out plate-frame filtering, sheet frame pressure≤0.3MPa, the filtrate warp of collection
Ceramic membrane filter, controls inlet pressure≤0.3MPa of film, and the outlet pressure 0.15-0.25MP of film enters back into ethyl alcohol after filtering
Destilling tower；
Step 3: ethyl alcohol being heated by steam, vapo(u)rizing temperature controls in 70-110 DEG C, 100-110 DEG C of column bottom temperature, tower
80-95 DEG C of temperature, 70-80 DEG C of tower top temperature, distillation treated alcohol gas is condensed through condenser and is received subsequently into collecting tank
Collection, wherein the control of condenser condensation temperature is at 50 DEG C or less.
Wherein calcium salt is one of calcium carbonate, calcium sulfate, calcium nitrate, calcium phosphate, calcium oxide, calcium hydroxide in step 1
Or it is several, magnesium salts is one or more of magnesium chloride, magnesium sulfate, magnesia, and alkaline solution is ammonium hydroxide, liquid alkaline, 20% sodium carbonate
One or more of.
Embodiment 2
The invention discloses the recovery methods of ethyl alcohol in aureomycin hydrochloride crystalline mother solution, and implementation steps are as described in Example 1,
It is as follows that parameter is embodied:
Take 10m3Aureomycin hydrochloride crystalline mother solution, through detecting, amount of alcohol 5.5m3.100kg calcium carbonate, stirring 10 is added
Minute.Adjusting pH with liquid alkaline is 7.0, is stirred 20 minutes.Through plate-frame filtering, pressure 0.25MPa collects filtrate again through film mistake
Filter, controls the inlet pressure 0.3MPa of film, the outlet pressure 0.25MPa of film is then fed into ethanol distillation tower.Destilling tower steams
Vapour heating, temperature control: 90-94 DEG C in 106-110 DEG C of tower bottom, tower, 76-80 DEG C of tower top.Distillation treated alcohol gas warp
Condenser is condensed to 30-40 DEG C, subsequently into collecting tank.Recycling terminates, and is collected into ethyl alcohol 5.4m3, ethanol content 94%.Mother liquor
The rate of recovery is 54%, ethanol recovery 92.3%.
Embodiment 3
The invention discloses the recovery methods of ethyl alcohol in aureomycin hydrochloride crystalline mother solution, and implementation steps are as described in Example 1,
It is as follows that parameter is embodied:
Take 10m3Aureomycin hydrochloride crystalline mother solution, through detecting, amount of alcohol 5.4m3.50kg calcium carbonate, 50kg chlorine is added
Change magnesium, stirs 20 minutes.Adjusting pH with ammonium hydroxide is 7.5, is stirred 10 minutes.Through plate-frame filtering, pressure 0.24MPa collects filter
Liquid is filtered through film again, controls the inlet pressure 0.25MPa of film, and the outlet pressure 0.2MPa of film is then fed into ethanol distillation tower.
Destilling tower is heated with steam, temperature control: 86-90 DEG C in 104-108 DEG C of tower bottom, tower, 72-76 DEG C of tower top.Treated for distillation
Alcohol gas is condensed through condenser to 40-50 DEG C, subsequently into collecting tank.Recycling terminates, and is collected into ethyl alcohol 5.3m3, ethyl alcohol contains
Amount 93%.Disposing mother liquor rate is 53%, ethanol recovery 91.3%.
Embodiment 4
The invention discloses the recovery methods of ethyl alcohol in aureomycin hydrochloride crystalline mother solution, and implementation steps are as described in Example 1,
It is as follows that parameter is embodied:
Take 10m3Aureomycin hydrochloride crystalline mother solution, through detecting, amount of alcohol 6.7m3.150kg calcium carbonate, stirring 15 is added
Minute.Adjusting pH with liquid alkaline is 8.0, is stirred 30 minutes.Through plate-frame filtering, pressure 0.22MPa collects filtrate again through film mistake
Filter, controls the inlet pressure 0.2MPa of film, the outlet pressure 0.15MPa of film is then fed into ethanol distillation tower.Destilling tower steams
Vapour heating, temperature control: 80-84 DEG C in 100-104 DEG C of tower bottom, tower, 70-74 DEG C of tower top.Distillation treated alcohol gas warp
Condenser is condensed to 30-40 DEG C, subsequently into collecting tank.Recycling terminates, and is collected into ethyl alcohol 6.6m3, ethanol content 92%.Mother liquor
The rate of recovery is 66%, ethanol recovery 90.6%.
Embodiment 5
Test objective and method: in order to optimize implementing process of the present invention and parameter, the present embodiment is in 1 method of embodiment as base
Plinth carries out parameter optimization for mother liquor neutralization pretreatment and the control of ethanol distillation tower temperature of each section.
Experimental result:
1 mother liquor neutralization pretreatment experiment parameter table of table
| Test group | Mother liquor volume | Calcium and magnesium salt (kg) | PH value | Disposing mother liquor rate (%) |
| Test 1 | 10m³ | 100 | 6.5 | 54 |
| Test 2 | 10m³ | 120 | 7.6 | 56 |
| Test 3 | 10m³ | 150 | 8.0 | 58 |
| Test 4 | 10m³ | 170 | 9.0 | 58 |
2 ethanol distillation tower temperature degree control and ethanol recovery relationship of table
| Column bottom temperature (DEG C) | Temperature (DEG C) in tower | Column bottom temperature (DEG C) | Ethanol recovery (%) |
| 103 | 82 | 73 | 91.2 |
| 105 | 83 | 74 | 92.4 |
| 107 | 85 | 75 | 92.8 |
| 109 | 86 | 77 | 92.4 |
As shown in table 1,2, it is can be found that by the optimal screening of mother liquor neutralization pretreatment experiment parameter as calcium and magnesium salt is used
Amount improves and the raising of pH value, disposing mother liquor rate are significantly improved, but with the raising of calcium and magnesium dosage and pH value, corresponding calcium
Magnesium salts and alkaline solution input cost increase, with 500 yuan/ton of calcium and magnesium salt or so, 5000 yuan/ton of ethyl alcohol cost or so, liquid alkaline at
This 800 yuan/ton or so progress cost accounting, using 3 input amount of test group as Optimal Input amount.
It is controlled by carrying out different temperature to ethanol distillation tower, it is found that in destilling tower, temperature of each section is mentioned
Height, ethanol recovery presentation first increase the experimental trend subtracted afterwards, and at 107 DEG C of column bottom temperature, 85 DEG C of temperature, tower top temperature in tower
Ethanol recovery reaches experiment peak for 92.8% at 75 DEG C.
Embodiment 6
Experiment purpose and method: in order to compare implementation method and conventional method of the present invention in aureomycin hydrochloride crystalline mother solution
Ethyl alcohol recovery efficiency, wherein conventional method is by 10m3Aureomycin hydrochloride mother liquor be sent directly into destilling tower；The method of the present invention is then
Implement by embodiment 2.
Experimental result:
Compared with the implementation method of the present invention of table 3. is recycled with conventional method ethyl alcohol
| Mother liquor volume | Conventional method | The present invention | The rate of recovery improves |
| 10m³ | 5.5 m3 | 5.8 m3 | 5.4% |
| 10m³ | 5.2 m3 | 5.4 m3 | 3.8% |
| 10m³ | 6.1 m3 | 6.5 m3 | 6.5% |
As shown in table 3, it is recycled by comparing implementation method of the present invention and conventional method ethyl alcohol, it can be found that identical handling
Under conditions of volume mother liquor, the ethanol recovery of implementation method of the present invention is higher, and energy consumption control is more accurate in the process, and cost is thrown
Enter lower.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.
Claims (3)
1. the recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution, which is characterized in that comprise the steps that
Step 1: aureomycin hydrochloride crystalline mother solution carries out neutralization pretreatment, forms suspension, continues stirring 10-30 minutes；
Step 2: the suspension that step 1 is obtained carries out plate-frame filtering, and sheet frame pressure≤0.3MPa, the filtrate of collection is through film mistake
Ethanol distillation tower is entered back into after filter；
Step 3: ethyl alcohol is heated by steam, vapo(u)rizing temperature is controlled at 70-110 DEG C, and carry out tower bottom, in tower, three temperature of tower top
Degree control, in the tower bottom, tower, three temperature controls of tower top be respectively 100-110 DEG C of column bottom temperature, temperature 80-95 in tower
DEG C, 70-80 DEG C of tower top temperature, distillation treated alcohol gas is condensed through condenser and is collected subsequently into collecting tank, wherein cold
Condenser condensation temperature is controlled at 50 DEG C or less；
Step 1 neutralization pretreatment is the calcium salt that addition mass-volume concentration is 0.5-5% or mass-volume concentration is 0-
6% magnesium salts stirs 10-30 minutes, with alkaline solution tune pH to 5.5-8.0, wherein the calcium salt is calcium carbonate, sulfuric acid
One or more of calcium, calcium nitrate, calcium phosphate, the magnesium salts be one or more of magnesium chloride, magnesium sulfate, it is described
Alkaline solution is one or more of ammonium hydroxide, liquid alkaline, 20% sodium carbonate.
2. the recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution as described in claim 1, it is characterised in that: the step
Film is filtered into using ceramic membrane filter in rapid 2, controls inlet pressure≤0.3MPa of film, the outlet pressure 0.15- of film
0.25MPa。
3. the recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution as described in claim 1, it is characterised in that: the calcium
Salt is calcium carbonate, and the magnesium salts is magnesium chloride, and the alkaline solution is liquid alkaline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610694184.5A CN106316794B (en) | 2016-08-22 | 2016-08-22 | The recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610694184.5A CN106316794B (en) | 2016-08-22 | 2016-08-22 | The recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106316794A CN106316794A (en) | 2017-01-11 |
| CN106316794B true CN106316794B (en) | 2019-02-26 |
Family
ID=57744445
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610694184.5A Active CN106316794B (en) | 2016-08-22 | 2016-08-22 | The recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106316794B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110294665B (en) * | 2019-07-09 | 2024-02-20 | 常州制药厂有限公司 | Recovery device and recovery method for ethanol in doxycycline hydrochloride refined mother liquor |
| CN114105804B (en) * | 2021-12-15 | 2023-09-15 | 浦城正大生化有限公司 | Preparation method of aureomycin hydrochloride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2871265A (en) * | 1956-09-27 | 1959-01-27 | American Cyanamid Co | Process for preparing chlortetracycline sulfate |
| GB1223962A (en) * | 1968-02-28 | 1971-03-03 | Diamond Shamrock Corp | Improvements in or relating to crystalline chlortetracycline bisulfate |
| CN103044196A (en) * | 2011-12-30 | 2013-04-17 | 宜昌三峡制药有限公司 | Lysine acetate mother liquid recycling method |
| CN103739514A (en) * | 2013-12-24 | 2014-04-23 | 福建省福抗药业股份有限公司 | Production method of chlortetracycline bisulfate |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6004321B2 (en) * | 2012-04-18 | 2016-10-05 | 日立造船株式会社 | Methods for controlling the growth of miscellaneous bacteria in ethanol fermentation of moss |
-
2016
- 2016-08-22 CN CN201610694184.5A patent/CN106316794B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2871265A (en) * | 1956-09-27 | 1959-01-27 | American Cyanamid Co | Process for preparing chlortetracycline sulfate |
| GB1223962A (en) * | 1968-02-28 | 1971-03-03 | Diamond Shamrock Corp | Improvements in or relating to crystalline chlortetracycline bisulfate |
| CN103044196A (en) * | 2011-12-30 | 2013-04-17 | 宜昌三峡制药有限公司 | Lysine acetate mother liquid recycling method |
| CN103739514A (en) * | 2013-12-24 | 2014-04-23 | 福建省福抗药业股份有限公司 | Production method of chlortetracycline bisulfate |
Non-Patent Citations (2)
| Title |
|---|
| 从强力霉素的转化母液中回收磺基水杨酸;包泉兴 等;《医药工业》;19821231;第42页第1段 |
| 用尿素乙醇结晶制取金霉素盐酸盐的工艺试验;裴文忠;《中国卫生产业》;20141231;第14页4 工艺方法，第16页左栏第1段 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106316794A (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109019691B (en) | Preparation process of ammonium paratungstate | |
| CN104370312B (en) | Recycling processing technology for high-salt wastewater during carboxymethyl cellulose production | |
| CN106316794B (en) | The recovery method of ethyl alcohol in aureomycin hydrochloride crystalline mother solution | |
| CN107235939B (en) | In a kind of aldehyde vapour gas phase and the method that improves furaldehyde yield | |
| CN206188408U (en) | Ammonium bicarbonate system device is retrieved to double tower negative pressure deamination | |
| CN101182079A (en) | Citric acid mother liquor treatment process | |
| CN101723845B (en) | Method for producing m-acetamino-N,N-diethyl aniline | |
| CN103467344B (en) | Method for recovering urea from tetracycline urea compound salt crystallization mother liquor and recycling urea | |
| CN115679128B (en) | Method for efficiently recovering tungsten and ammonia from tungsten-containing dephosphorization precipitated slag | |
| CN104743694B (en) | Recycling processing method and device of heavy metal ion-containing organic acid wastewater | |
| CN110194715A (en) | A kind of production method of sodium formate | |
| CN106699591A (en) | Clean production process of glycine and co-produced ammonium chloride | |
| CN103274923B (en) | Method for recycling dehydropregnenolone acetate waste liquor | |
| CN101550063A (en) | Method for purifying ultra-purity absolute ethyl alcohol | |
| RU2517524C2 (en) | Method and apparatus for processing hydrogen in purification unit of terephthalic acid purification device | |
| CN104524797B (en) | Energy-conservation concentration and evaporation method in zirconium oxychloride production process | |
| CN106977442A (en) | A kind of extraction process of hydroxyproline | |
| CN112607772A (en) | Method for extracting high-purity titanium dioxide from olefin polymerization industrial waste acid residues | |
| CN210449119U (en) | Resin polymerization reaction system | |
| CN204490660U (en) | A kind of novel dyeing waste water total system | |
| CN210419811U (en) | Amine alcohol compound reaction system | |
| CN104710046B (en) | A kind of novel rare-earth wastewater comprehensive treatment system and method | |
| CN211987148U (en) | Fractionating device for mixed acid of phosphoric acid, acetic acid and nitric acid | |
| CN103030183B (en) | Device and method for recycling waste water for washing plate frame for pentaerythritol | |
| CN109896683A (en) | The cycling and reutilization treatment process of time acid producing waste water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |