CN101781198A - Technology for recovering mother solution of gallic acid - Google Patents
Technology for recovering mother solution of gallic acid Download PDFInfo
- Publication number
- CN101781198A CN101781198A CN200910226622A CN200910226622A CN101781198A CN 101781198 A CN101781198 A CN 101781198A CN 200910226622 A CN200910226622 A CN 200910226622A CN 200910226622 A CN200910226622 A CN 200910226622A CN 101781198 A CN101781198 A CN 101781198A
- Authority
- CN
- China
- Prior art keywords
- gallic acid
- technology
- mother solution
- solution
- filtrate
- 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.)
- Granted
Links
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229940074391 gallic acid Drugs 0.000 title claims abstract description 33
- 235000004515 gallic acid Nutrition 0.000 title claims abstract description 33
- 238000005516 engineering process Methods 0.000 title claims abstract description 10
- 239000010413 mother solution Substances 0.000 title claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000004062 sedimentation Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000012452 mother liquor Substances 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 6
- 238000011084 recovery Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 abstract 3
- 238000001035 drying Methods 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses technology for recovering other solution of gallic acid, which comprises the following steps: adding NaOH or CaO into the mother solution for stirring; regulating the pH of the solution to between 8.5 and 9.0; performing centrifugal sedimentation and filtering, drying the filtrate at the temperature of between 40 and 55 DEG C, and obtaining a coarse product of the gallic acid; and centrifuging by using a centrifugal machine, settling for 2 hours, filtering and drying the filtrate at 50 DEG C, and obtaining a coarse product of the gallic acid. The recovery percent of the mother solution of the gallic acid can reach over 80 percent, and the rate of reducing the filtrate CODcr can reach over 90 percent. Meanwhile, the technology is simple, and the emission of harmful substances can be effectively reduced.
Description
Technical field
The present invention relates to a kind of fine chemical product gallic acid and produce depleted crystalline mother solution recovery technology and method.
Background technology
Turkey-galls is China's characteristic biochemical industry resource, China's Turkey-galls processing industry overall technology level also is in the primary stage at present, the rough crystalline mother solution that discharges in the processing gallic acid particularly, the organic concentration height, gallic acid content reaches 0.9%-1.5%, the discarded thick mother liquor water quality detection chemical oxygen demand (COD) (CODcr) of gallic acid reaches 42427mg/L, five-day BOD (BOD
5) 24358mg/L, ammonia nitrogen 2942mg/L, the social danger that water surrounding in the basin and people's lives are caused is big, and it is difficult to administer.Present family surplus the existing Turkey-galls processing enterprise 20 in the whole nation, ton, the wherein surplus ton of CODcr2460 surplus the ton surplus year processing Turkey-galls 5000, estimation year discharging high-concentration industrial-water 65000; Waste water is taken away ton surplus the product 580 such as gallic acid, about 6,467 ten thousand yuan of financial loss.Reinforcement has its vital role to the recycling treatment and the recovery of its high-concentration waste water source of pollution mother solution of gallic acid for industry discharged wastewater met the national standard.
Summary of the invention
The object of the present invention is to provide a kind of recovery processing technique of mother solution of gallic acid, by to different concns gallic acid aqueous solution COD, BOD
5Gallic acid content and COD concentration are closely related and linear in the detection discovery waste water, as long as reclaim object gallic acid in the mother liquor, just can reduce COD in the mother liquor, BOD greatly
5Content.
Technology of the present invention may further comprise the steps:
Get mother liquor and add NaOH or CaO stirring, transfer to PH=8.5-9.0, centrifugal settling is filtered, and 40-55 ℃ of oven dry of filter thing obtains the gallic acid crude product; Whizzer is centrifugal, and sedimentation 2h filters, and 50 ℃ of oven dry of filter thing get the gallic acid crude product.
The mother liquor gallic acid rate of recovery of the present invention can reach more than 80%, and liquor C ODcr reduced rate can reach more than 90%.And technology is simple, can effectively reduce emission of harmful substances.
Embodiment
Embodiment 1:
Get gallic acid crystallization centrifuge mother liquor 500ml, mother liquor PH instrumentation pH value 1.3, high performance liquid chromatograph detects gallic acid content 0.9155mg/ml, and CODcr measures 36300mg/L.Mother liquor places the 1000ml beaker, adds caustic soda (NaOH), and magnetic stirrer stirs, and transfers pH value to 8.0, spends caustic soda (NaOH) 21.5 grams.Whizzer is centrifugal, and sedimentation 2h filters, and gets supernatant liquor HPLC method check gallic acid content 0.3417mg/ml, and CODcr measures 12600mg/L, CODcr reduced rate 65.28%.50 ℃ of oven dry of filter thing get gallic acid crude product 272.5mg, and high performance liquid chromatograph detects gallic acid purity 76.2%, content 207.6mg, the gallic acid rate of recovery 45.35%.
Embodiment 2:
Get gallic acid crystallization centrifuge mother liquor 500ml, mother liquor PH instrumentation pH value 1.3, high performance liquid chromatograph detects gallic acid content 0.9645mg/ml, and CODcr measures 36800mg/L.Mother liquor places the 1000ml beaker, adds lime (CaO), and magnetic stirrer stirs, and transfers pH value to 8.5, with delime (CaO) 22.5 grams.Whizzer is centrifugal, and sedimentation 20min filters, and gets supernatant liquor HPLC method check gallic acid content 0.0325mg/ml, and CODcr measures 2400mg/L, CODcr reduced rate 93.47%.50 ℃ of oven dry of filter thing get gallic acid crude product 623.9mg, and high performance liquid chromatograph detects gallic acid purity 68.5%, content 207.6mg, the gallic acid rate of recovery 88.62%.
Claims (1)
1. a technology for recovering mother solution of gallic acid is characterized in that, comprising: get mother liquor and add NaOH or CaO stirring, transfer to PH=8.5-9.0, centrifugal settling is filtered, and 40-55 ℃ of oven dry of filter thing obtains the gallic acid crude product; Whizzer is centrifugal, and sedimentation 2h filters, and 50 ℃ of oven dry of filter thing get the gallic acid crude product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910226622 CN101781198B (en) | 2009-12-10 | 2009-12-10 | Technology for recovering mother solution of gallic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910226622 CN101781198B (en) | 2009-12-10 | 2009-12-10 | Technology for recovering mother solution of gallic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101781198A true CN101781198A (en) | 2010-07-21 |
| CN101781198B CN101781198B (en) | 2013-01-30 |
Family
ID=42521364
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910226622 Active CN101781198B (en) | 2009-12-10 | 2009-12-10 | Technology for recovering mother solution of gallic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101781198B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778974A (en) * | 2016-05-11 | 2016-07-20 | 西南石油大学 | Recovery device for CO2 switchable solvent for processing oil-based drilling cuttings |
| CN107180662A (en) * | 2017-06-23 | 2017-09-19 | 中国核动力研究设计院 | AUGdC mother liquor of precipitation of ammonium recovery processing techniques |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1706790A (en) * | 2005-05-09 | 2005-12-14 | 竹山县天新医药化工有限责任公司 | Gallic acid producing process |
| CN101161597A (en) * | 2006-07-24 | 2008-04-16 | 乐山三江生化科技有限公司 | Purifying recovery method of gallic acid production wastewater |
-
2009
- 2009-12-10 CN CN 200910226622 patent/CN101781198B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1706790A (en) * | 2005-05-09 | 2005-12-14 | 竹山县天新医药化工有限责任公司 | Gallic acid producing process |
| CN101161597A (en) * | 2006-07-24 | 2008-04-16 | 乐山三江生化科技有限公司 | Purifying recovery method of gallic acid production wastewater |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778974A (en) * | 2016-05-11 | 2016-07-20 | 西南石油大学 | Recovery device for CO2 switchable solvent for processing oil-based drilling cuttings |
| CN105778974B (en) * | 2016-05-11 | 2017-05-03 | 四川奎能环保科技有限公司 | Recovery device for CO2 switchable solvent for processing oil-based drilling cuttings |
| CN107180662A (en) * | 2017-06-23 | 2017-09-19 | 中国核动力研究设计院 | AUGdC mother liquor of precipitation of ammonium recovery processing techniques |
| CN107180662B (en) * | 2017-06-23 | 2019-03-01 | 中国核动力研究设计院 | AUGdC mother liquor of precipitation of ammonium recovery processing technique |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101781198B (en) | 2013-01-30 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
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| CP01 | Change in the name or title of a patent holder |
Address after: 427000 Xixi Zhangjiajie economic and Technological Development Zone, Yongding District, Zhangjiajie, Hunan Patentee after: JIURUI BIOLOGY & CHEMISTRY CO.,LTD. Address before: 427000 Xixi Zhangjiajie economic and Technological Development Zone, Yongding District, Zhangjiajie, Hunan Patentee before: ZHANGJIAJIE AOWEI SCIENCE & TECHNOLOGY Co.,Ltd. |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Gallic acid mother liquor recovery process Effective date of registration: 20230628 Granted publication date: 20130130 Pledgee: Bank of Communications Co.,Ltd. Zhangjiajie branch Pledgor: JIURUI BIOLOGY & CHEMISTRY CO.,LTD. Registration number: Y2023980046143 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Granted publication date: 20130130 Pledgee: Bank of Communications Co.,Ltd. Zhangjiajie branch Pledgor: JIURUI BIOLOGY & CHEMISTRY CO.,LTD. Registration number: Y2023980046143 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Recovery and treatment process of gallic acid mother liquor Granted publication date: 20130130 Pledgee: Bank of Communications Co.,Ltd. Zhangjiajie branch Pledgor: JIURUI BIOLOGY & CHEMISTRY CO.,LTD. Registration number: Y2024980025097 |