CN107673511A - A kind of tower draws chinic acid recovery method in standby gallic acid waste liquid - Google Patents
A kind of tower draws chinic acid recovery method in standby gallic acid waste liquid Download PDFInfo
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- CN107673511A CN107673511A CN201711114905.1A CN201711114905A CN107673511A CN 107673511 A CN107673511 A CN 107673511A CN 201711114905 A CN201711114905 A CN 201711114905A CN 107673511 A CN107673511 A CN 107673511A
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- waste liquid
- acid
- chinic
- standby
- chinic acid
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of tower to draw chinic acid recovery method in standby gallic acid waste liquid, gallic acid waste liquid quiescent settling is removed into mechanicalness impurity first, then impurity is further removed by ceramic membrane, waste liquid passes through the first selective recovery gallic acid of resin after removal of impurities, then waste liquid is passed through into NF membrane, reduce salinity in waste water, the waste liquid of low salt concn be can obtain into chinic acid crude product by resin adsorption desorption again, re-refine to obtain purity and reach more than 80% up to more than 95% chinic acid, organic efficiency.Its energy recovery tower draws the chinic acid in standby gallic acid waste liquid, avoids the wasting of resources, while reduces the COD in waste liquid, reduces sewage disposal difficulty.
Description
Technical field
The invention belongs to Chemical Manufacture, the utilization of resources and environmental protection technical field, and in particular to a kind of tower is drawn for not having
Chinic acid recovery method in infanticide acid waste liquid.
Background technology
Chinic acid is a kind of fine chemical product and medicine intermediate with high value, in medicine, food, chemical industry etc.
Industry has a wide range of applications.Its partial derivatives has been found a variety of important pharmacological actions, such as shikimic acid, green original
Acid, caffeoyl guinic acid and anti-influenza medicament oseltamivir phosphate are the derivatives of chinic acid.Chinic acid is plant aerobic respiration process
In, the one kind formed by shikimic acid pathway has optically active cyclic polyhydroxy compound.The chinic acid production in China at present
Substantially or blank, whole rely on imports.
The talas of tannic acid of China's hydrolysis at present obtains the production technology of gallic acid also in " resource-product-pollution is arranged
Put " material one-way road on, this had not both met the core requirement of present Green Chemistry, at the same for company and it is a kind of greatly
The wasting of resources, proportion of the chinic acid in talas of tannic acid is 15%-17% or so, is had equivalent to every one ton of gallic acid of production
190kg or so chinic acid is lost in sewage, and the chinic acid market price is annual raw with one at 150,000 yuan/ton or so at present
The producer of 2000 tons of gallic acids of production calculates, every year with i.e. up to 60,000,000 yuan or so of the chinic acid loss of sewage discharge.
The industrialization that chinic acid reclaims in standby gallic acid waste liquid is drawn there has been no tower report that the invention of this method has at present
The blank for having filled up this aspect of effect, great commercial value.
The content of the invention
The purpose of the present invention is to be directed to problem above, there is provided a kind of tower draws chinic acid recovery side in standby gallic acid waste liquid
Method, its energy recovery tower draws the chinic acid in standby gallic acid waste liquid, avoids the wasting of resources, while reduces the COD in waste liquid, drops
Low sewage disposal difficulty.
To realize the purpose, this method employs following steps to the chinic acid in recovery gallic acid waste liquid：
（1）, mechanical admixture in gallic acid waste liquid is removed using sedimentation method, then further removed using ceramic membrane filter
The organic impurities of larger molecular weight, obtain sedimentation waste liquid；
（2）, using the gallic acid in ion exchange resin adsorption and sedimentation waste liquid, reclaimed, obtain removal of impurities waste liquid；
（3）, utilize nanofiltration membrane removal of impurities waste liquid so that salinity obtains low-salt-content liquid waste to 0.2-0.5% in removal of impurities waste liquid；
（4）, using the chinic acid in the adsorption-desorption effect recovery low-salt-content liquid waste of polymeric adsorbent, obtain chinic acid crude product；By Kui Buddhist nun
Acid crude be refining to obtain the chinic acid of high-purity.
Preferably, step（4）In polymeric adsorbent be acrylic acid series weak-base ion-exchange resin, the resin includes primary
Amino or pyridine radicals.
Preferably, step（4）In polymeric adsorbent be HPS355 or ND900 resins.
Preferably, step（4）In, it is water-soluble that hydrochloric acid of the resin of chinic acid successively with pure water and various concentrations will be adsorbed with
Liquid washs, and collects cleaning solution, is then transferred in Rotary Evaporators and is evaporated, obtain chinic acid crude product.
Preferably, step（4）In, the refined method of chinic acid is recrystallization, and solvent used is that methanol or ethanol are water-soluble
Liquid.
Preferably, step（4）In the refined method of middle chinic acid, the chinic acid crude product activated carbon decolorizing that will first obtain,
Then to be purified again with the method for recrystallization, recrystallization solvent for use is the methanol or ethanol water of different quality number concentration,
Its mass fraction concentration range is 10%-50%.
Beneficial effects of the present invention：
Its energy recovery tower draws the chinic acid in standby gallic acid waste liquid, avoids the wasting of resources, while reduces the COD in waste liquid,
Reduce sewage disposal difficulty.
Brief description of the drawings
Fig. 1 is the preparation technology process principle figure of the present invention.
Embodiment
In order that those skilled in the art more fully understand technical scheme, the present invention is entered below in conjunction with the accompanying drawings
Row is described in detail, and the description of this part is only exemplary and explanatory, should not there is any limitation to protection scope of the present invention
Effect.
As shown in figure 1, the concrete technology flow process of the present invention is：
To realize the purpose, this method employs following steps to the chinic acid in recovery gallic acid waste liquid：
（1）, mechanical admixture in gallic acid waste liquid is removed using sedimentation method, then further removed using ceramic membrane filter
The organic impurities of larger molecular weight, obtain sedimentation waste liquid；
（2）, using the gallic acid in ion exchange resin adsorption and sedimentation waste liquid, reclaimed, obtain removal of impurities waste liquid；
（3）, utilize nanofiltration membrane removal of impurities waste liquid so that salinity obtains low-salt-content liquid waste to 0.2-0.5% in removal of impurities waste liquid；
（4）, using the chinic acid in the adsorption-desorption effect recovery low-salt-content liquid waste of polymeric adsorbent, obtain chinic acid crude product；By Kui Buddhist nun
Acid crude be refining to obtain the chinic acid of high-purity.
Preferably, step（4）In polymeric adsorbent be acrylic acid series weak-base ion-exchange resin, the resin includes primary
Amino or pyridine radicals.
Preferably, step（4）In polymeric adsorbent be HPS355 or ND900 resins.
Preferably, step（4）In, it is water-soluble that hydrochloric acid of the resin of chinic acid successively with pure water and various concentrations will be adsorbed with
Liquid washs, and collects cleaning solution, is then transferred in Rotary Evaporators and is evaporated, obtain chinic acid crude product.
Preferably, step（4）In, the refined method of chinic acid is recrystallization, and solvent used is that methanol or ethanol are water-soluble
Liquid.
Preferably, step（4）In the refined method of middle chinic acid, the chinic acid crude product activated carbon decolorizing that will first obtain,
Then to be purified again with the method for recrystallization, recrystallization solvent for use is the methanol or ethanol water of different quality number concentration,
Its mass fraction concentration range is 10%-50%.
The principle of the invention：
Gallic acid waste liquid quiescent settling is removed into mechanicalness impurity first, impurity is further then removed by ceramic membrane, removed
Waste liquid then by waste liquid by NF membrane, reduces salinity in waste water by the recovery gallic acid of the first selectivity of resin after miscellaneous,
The waste liquid of low salt concn be can obtain into chinic acid crude product by resin adsorption-desorption again, re-refine to obtain purity up to more than 95%
Chinic acid, organic efficiency reaches more than 80%.
Embodiment：
Sedimentation, the waste liquid that tower drawing hydrolysis is prepared to gallic acid are transferred to settling tank, make the mechanicalness impurity sedimentation in waste liquid abundant.
Ceramic membrane cleans, and will settle sufficient waste liquid by ceramic membrane, further remove in waste liquid larger particles impurity or
Larger molecular organicses.
Resins selective adsorbs gallic acid, can be with selective absorption waste liquid by HPS355 or ND900 resins by waste liquid
In gallic acid and larger molecular organicses such as tannic acid etc., adsorption efficiency reaches more than 95%.
Salinity is reduced, after waste liquid removes the main organic matter such as gallic acid by resin, waste liquid is passed through into NF membrane, drop
Its low salinity, its salt concentration range are controlled in 0.2%-0.5%.
Resin adsorption chinic acid, gallic acid waste liquid of the salinity between 0.2%-0.5% is passed through into acrylic acid series weak base
Property ion exchange resin（Resin includes primary amino radical or pyridine radicals）.
Chinic acid desorption, the resin for being adsorbed with chinic acid is washed with the aqueous hydrochloric acid solution of pure water and various concentrations successively
Wash, collect cleaning solution, be then transferred in Rotary Evaporators and be evaporated, produce chinic acid crude product.
Chinic acid is refined, and obtained chinic acid crude product is first used into activated carbon decolorizing, is then purified again with the method for recrystallization,
The methanol or ethanol water that solvent for use is various concentrations are recrystallized, its concentration range is between 10%-50%.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
And also include the other element being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
Specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example
It is only intended to help the method and its core concept for understanding the present invention.Described above is only the preferred embodiment of the present invention, should
When pointing out due to the finiteness of literal expression, and unlimited concrete structure objectively be present, for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, some improvement, retouching or change can also be made, can also incited somebody to action
Above-mentioned technical characteristic is combined by rights；These improve retouching, change or combination, or the not improved structure by invention
Think and technical scheme directly applies to other occasions, be regarded as protection scope of the present invention.
Claims (6)
1. a kind of tower draws chinic acid recovery method in standby gallic acid waste liquid, it is characterised in that it includes step is produced by below：
（1）, mechanical admixture in gallic acid waste liquid is removed using sedimentation method, then further removed using ceramic membrane filter
The organic impurities of larger molecular weight, obtain sedimentation waste liquid；
（2）, using the gallic acid in ion exchange resin adsorption and sedimentation waste liquid, reclaimed, obtain removal of impurities waste liquid；
（3）, utilize nanofiltration membrane removal of impurities waste liquid so that salinity obtains low-salt-content liquid waste to 0.2-0.5% in removal of impurities waste liquid；
（4）, using the chinic acid in the adsorption-desorption effect recovery low-salt-content liquid waste of polymeric adsorbent, obtain chinic acid crude product；By Kui Buddhist nun
Acid crude be refining to obtain the chinic acid of high-purity.
2. a kind of tower according to claim 1 draws chinic acid recovery method in standby gallic acid waste liquid, it is characterised in that
Step（4）In polymeric adsorbent be acrylic acid series weak-base ion-exchange resin, the resin includes primary amino radical or pyridine radicals.
3. a kind of tower according to claim 2 draws chinic acid recovery method in standby gallic acid waste liquid, it is characterised in that
Step（4）In polymeric adsorbent be HPS355 or ND900 resins.
4. a kind of tower according to claim 1 draws chinic acid recovery method in standby gallic acid waste liquid, it is characterised in that
Step（4）In, the resin for being adsorbed with chinic acid is washed with the aqueous hydrochloric acid solution of pure water and various concentrations successively, collects washing
Liquid, then it is transferred in Rotary Evaporators and is evaporated, obtains chinic acid crude product.
5. a kind of tower according to claim 1 draws chinic acid recovery method in standby gallic acid waste liquid, it is characterised in that
Step（4）In, the refined method of chinic acid is recrystallization, and solvent used is methanol or ethanol water.
6. a kind of tower according to claim 5 draws chinic acid recovery method in standby gallic acid waste liquid, it is characterised in that
Step（4）In the refined method of middle chinic acid, the chinic acid crude product activated carbon decolorizing that will first obtain, then again with recrystallization
Method purifies, and recrystallizes methanol or ethanol water that solvent for use is different quality number concentration, its mass fraction concentration model
Enclose for 10%-50%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711114905.1A CN107673511A (en) | 2017-11-13 | 2017-11-13 | A kind of tower draws chinic acid recovery method in standby gallic acid waste liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711114905.1A CN107673511A (en) | 2017-11-13 | 2017-11-13 | A kind of tower draws chinic acid recovery method in standby gallic acid waste liquid |
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| CN107673511A true CN107673511A (en) | 2018-02-09 |
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| CN201711114905.1A Pending CN107673511A (en) | 2017-11-13 | 2017-11-13 | A kind of tower draws chinic acid recovery method in standby gallic acid waste liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574924A (en) * | 2019-01-16 | 2019-04-05 | 浙江国邦药业有限公司 | A kind of Enrofloxacin raffinate recoverying and utilizing method |
| CN114426264A (en) * | 2021-12-24 | 2022-05-03 | 天津环渤新材料有限公司 | Electronic acid waste liquid pretreatment module and electronic acid waste liquid recovery treatment method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5611931A (en) * | 1995-07-31 | 1997-03-18 | Media And Process Technology Inc. | High temperature fluid separations using ceramic membrane device |
| CN101265278A (en) * | 2008-04-25 | 2008-09-17 | 南京龙源天然多酚合成厂 | Method for preparing high-purity tarra edible tannic acid |
| CN102924268A (en) * | 2012-11-29 | 2013-02-13 | 云南瑞宝生物科技有限公司 | Method for preparing gallic acid |
-
2017
- 2017-11-13 CN CN201711114905.1A patent/CN107673511A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5611931A (en) * | 1995-07-31 | 1997-03-18 | Media And Process Technology Inc. | High temperature fluid separations using ceramic membrane device |
| CN101265278A (en) * | 2008-04-25 | 2008-09-17 | 南京龙源天然多酚合成厂 | Method for preparing high-purity tarra edible tannic acid |
| CN102924268A (en) * | 2012-11-29 | 2013-02-13 | 云南瑞宝生物科技有限公司 | Method for preparing gallic acid |
Non-Patent Citations (2)
| Title |
|---|
| 何国庆: "《食品发酵与酿造工艺学》", 31 August 2003 * |
| 周道兵等: "塔拉单宁水解废液回收奎尼酸的工艺试验", 《林产化工通讯》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574924A (en) * | 2019-01-16 | 2019-04-05 | 浙江国邦药业有限公司 | A kind of Enrofloxacin raffinate recoverying and utilizing method |
| CN114426264A (en) * | 2021-12-24 | 2022-05-03 | 天津环渤新材料有限公司 | Electronic acid waste liquid pretreatment module and electronic acid waste liquid recovery treatment method |
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