CN1057255A - Utilize tower to draw powder to produce gallic acid - Google Patents
Utilize tower to draw powder to produce gallic acid Download PDFInfo
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- CN1057255A CN1057255A CN 91102322 CN91102322A CN1057255A CN 1057255 A CN1057255 A CN 1057255A CN 91102322 CN91102322 CN 91102322 CN 91102322 A CN91102322 A CN 91102322A CN 1057255 A CN1057255 A CN 1057255A
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Abstract
A kind of tower that utilizes draws powder to produce the production technology of gallic acid.Generally, produce gallic acid system and adopt acid system production, the present invention adopts tower to draw powder (Tara powder) alkaline process to produce gallic acid, and proportioning raw materials, production and processing condition are conducted a research, the employing alkali hydrolysis method is produced, the advanced cost of technology is low, and low in the pollution of the environment, can replace Chinese gallotanninic acid, production technology of the present invention, with respect to tower draw raw material analyse pure after, the smart crystalline product rate of gallic acid can reach 71-72%, accounts for the 75-77% of coarse crystallization product.
Description
The present invention relates to a kind of organic chemical industry's production technology, specifically a kind of technology of drawing powder production gallic acid from tower.
Gallic acid, have another name called doubly acid, chemical name is 3,4, the 5-trihydroxybenzoic acid, English Gallic Acid by name, molecular weight is 188.14, white, needle-shaped crystals, be soluble in hot water, ethanol, glycerine, be insoluble to chloroform and benzene, content is more than 99%, and it is mainly used in medicine industry, foodstuffs industry and electronic industry.Generally, producing gallic acid is that Chinese gallotanninic acid is made raw material, adopts acid system production, complex manufacturing, and the cost height, contaminate environment, and also raw material sources lack.
The objective of the invention is to select for use a kind of alternative Chinese gallotanninic acid to produce the raw material of gallic acid and simplify production technique, reduce production costs, reduce the production technology of environmental pollution.
It is raw material that realization the present invention seeks to draw powder with tower, adopts two kinds of hydrolysis method to produce gallic acid.
The present invention has reduced production cost, has reduced environmental pollution, and product yield and purity are all higher, and remarkable economic efficiency is arranged, and have opened up raw material sources, has guaranteed the market supply of gallic acid.
The main raw material tower draws; be Caesalpinia spinosaKuntze (Caesalpinia Spinosa); its Weibull average content is 44.3%; its main product is in South America; this tara tannin acid is contained in the beanpod of Caesalpinia spinosaKuntze; be characterized in galloyl and the esterification of D-quinic acid and produce, tara tannin derive from free carboxyl in the quinic acid than peracidity, produce a molecule quinic acid and 4-5 gallic acid after the Caesalpinia spinosaKuntze hydrolysis:
Produce gallic acid though on producing, can adopt two kinds of alkali hydrolysis methods, its main processes is still hydrolysis, and its a kind of basic condition is to draw powder and liquid caustic soda to stir together in the raw material tower, and is warming up to 100-110 ℃, hydrolysis 1-2 hour, after filtration, the coarse crystallization thing is separated out in the filtrate cooling, refilters washing, filter cake adds water, add gac, obtain the gallic acid elaboration through refining, but yield is not as another kind of alkali hydrolysis method height.
The technological process and the process control condition of another kind of alkali hydrolysis method are divided into: draw powder to extract with 1: 10 water of bath raio to the raw material tower, extract liquid with the 2nd time and carry out the 1st extraction, 50-65 ℃ is down extracted 5-7 hour, extract for the 2nd time to adopt the water extracting, 50-65 ℃ following extracting 2-4 hour; Second decimation liquid all separates with the precipitate and separate device, and filtrate was staticly settled more than 24 hours, the impurity precipitation that the precipitate and separate device can not be removed; The smart filtration promptly uses pressure filter to filter, and gets the middle and lower part clarified liq, adds diatomite, filters with pressure filter again; Make clear liquid be concentrated into Be26, concentrated solution acquisition amount is 130% of a former charging capacity; The caustic alkali that adds 40-50% concentration to concentrated solution, have bubble during interpolation, care should be used to is careful, more takes care during particularly near neutrality, adds the back at 100-105 ℃ of following hydrolysis 1-6 hour, be neutralized to PH=6-7 with concentration 62.53% sulfuric acid (also available hydrochloric acid), re-adjustment PH=1.5-2.0 with the cooling of water jacket method of cooling or vacuum method and should make between temperature keeps 20-30 ℃, then has crystal to separate out, if temperature is reduced to below 20 ℃, then also have sodium chloride crystal and separate out; Use the bottom to discharge the formula separating centrifuge and separate, obtain coarse crystallization product (moisture 10%); By the coarse-grain product: water=1: 5 coarse-grain product that is dissolved in water, and press the coarse-grain product: gac=5: 1.5 adds gac, and add an amount of bariumchloride and EDTA, decolour down at 90-95 ℃ then and handled 1-2 hour, add diatomite before filtering, filter down in 90 ℃ with separating centrifuge, filtrate is separated out crystallization under the vacuum, after the centrifugation, with less water (about amount of solid 1.3%) washing leaching cake (crystal), filtrate is recycled to be extracted dog-house and does to extract liquid usefulness for the first time, and filter cake carries out vacuum-drying with promise tower solid blender, when from drying machine, taking out crystallization, should be by the oscillatory type agitator of bottom use.The smart crystalline product 3,4 that obtains, 5-trihydroxy methyl phenylformic acid ratio defective product accounts for the 71-72% after tower draws raw material pure, accounts for the 75-77% of coarse crystallization product.
Embodiment 1: product batch number 9012045
Drop into tower and draw powder 1200kg, add water 12M
3, extracting is 6 hours in the time of 60 ℃, and extract is separated with the precipitate and separate device, the filtrate that obtains was staticly settled 24 hours, get the middle and lower part clarified liq, add an amount of diatomite, re-use pressure filter and filter, the clear liquid after filtering is concentrated into Be26, can get 1540 liters of clear liquids; In this clear liquid, add 48% NaOH560 liter,, be neutralized to PH=6-7 for 720 liters, re-adjustment PH=1.5-2.0 with the sulfuric acid of Be50 105 ℃ of following basic hydrolysiss 6 hours; There is crystal to separate out 24 ℃ of temperature in following 21 hours; After filtration, get coarse crystallization thing 495kg, account for tower and draw 41.25% of material quantity; The coarse crystallization thing is added 2500 premium on currency and gac 150kg, 90 ℃ of decolourings 2 hours, and at 90 ℃ of following filtration dryings, 3,4, the smart crystalline product of 5-trihydroxybenzoic acid 380kg, accounting for tower, to draw raw material to roll over scalar 71.46%, accounts for 76.8% of coarse crystallization.
Embodiment 2: product batch number 9012050
Drop into tower and draw powder 1200kg, add water 12M
3, extracting is 6 hours in the time of 60 ℃, and extract is separated with the precipitate and separate device, and filtrate was staticly settled 24 hours, gets the middle and lower part clarified liq, adds an amount of diatomite, re-uses pressure filter and carries out the essence filtration; Clear liquid after filtering is concentrated into Be26, can obtains 1530 liters of clear liquids, add 545 liters of 48% liquid caustic soda in this clear liquid, basic hydrolysis 6 hours is neutralized to PH=6-7 for 740 liters, re-adjustment PH=1.0-2.0 with the sulfuric acid of Be50 concentration; There is crystal to separate out 24 ℃ of temperature in following 20 hours; After filtration, get coarse crystallization thing 505kg, account for 42.10% of the raw material tower amount of drawing; This coarse crystallization thing is added 2530 liters, add gac 151kg, 91 ℃ of decolourings 2 hours; And at 91 ℃ of following filtration dryings, 3,4, the smart crystalline product of 5-trihydroxybenzoic acid 382kg accounts for the raw material tower and draws and analyse scalarly 71.86%, accounts for 75.64% of coarse crystallization thing.
Drop into tower and draw powder 1200kg, add water 12M
3, 60 ℃ of extractings 6 hours, extract is separated with the precipitate and separate device, filtrate was staticly settled 24 hours, get the middle and lower part clarified liq, add an amount of diatomite, re-use pressure filter and carry out the essence filtration; Clear liquid after filtering is concentrated into Be26, can obtains 1570 liters of clear liquids, add 575 liters of 48% liquid caustic soda in this clear liquid, basic hydrolysis 6 hours is neutralized to PH=6-7 for 735 liters, re-adjustment PH=1.0-2.0 with the sulfuric acid of Be50 concentration; There is crystal to separate out 25 ℃ of temperature in following 23 hours; After filtration, get coarse crystallization thing 491kg, account for 40.92% of the raw material tower amount of drawing; This coarse crystallization thing is added 2500 premium on currency, adds gac 149kg, 92 ℃ of decolourings 2 hours, and at 92 ℃ of following filtration dryings, 3,4, the smart crystalline product 375kg of 5-trihydroxybenzoic acid accounts for the raw material tower and draws and analyse scalarly 70.54%, accounts for 76.38% of coarse crystallization thing.
Claims (4)
1, a kind of tower that utilizes draws powder to produce the production technology of gallic acid (have another name called doubly acid, chemical name are 3,4,5-trihydroxybenzoic acid), it is characterized in that utilizing containing Weibull and drawing powder to be raw material greater than 44.0% tower, with two kinds of alkali hydrolysis methods production gallic acids.
2, by the described gallic acid production technology of claim 1, the feature of its a kind of alkali hydrolysis method is that its main processes is hydrolysis, is to draw powder and alkali lye to feed intake in tower, stirs together and is warming up to 100-110 ℃, hydrolysis 1-2 hour, after filtering, coarse crystallization is separated out in the filtrate cooling, adds water again, add activated carbon decolorizing, filter, concentrate, cooling and the smart crystalline product of gallic acid;
3, by the described gallic acid production technology of claim 1, the feature of its another kind of alkali hydrolysis method is after drawing powder to feed intake in tower, continuously through the water extracting, separate, staticly settle, filter, concentrate, add that liquid caustic soda decomposes, neutralization, again transfer pH value, partial crystallization (make with extra care), separate coarse-grain, dissolve decolouring, filtration, partial crystallization, separation, drying process, obtain smart crystalline gallic acid product;
4, by claim 1 and 3 described gallic acid production technologies, it is characterized in that drawing powder by 1: 10 water of bath raio extraction, do to extract tower for the first time and draw powder, extract 5-7 hour down at 50-60 ℃ to extract for the second time liquid to the raw material tower, water extracts for the second time, and 50-65 ℃ is extracted 2-4 hour down; Extract after the separation staticly settled 24 hours, precipitated impurities; Add diatomite in the clear liquor after the filtration; The NaOH that in concentrated solution, adds 40-50% concentration, at 105-100 ℃ of following hydrolysis 1-6 hour, and be neutralized to PH=6-7 with sulfuric acid (or hydrochloric acid), re-adjustment PH=1.5-2.0, cooling also makes temperature remain on 20-30 ℃, separate out crystal, get the coarse crystallization product after the centrifuging, then by coarse-grain: water=be dissolved in water at 1: 5, and press coarse-grain: gac=5: 1.5 adding gacs, add an amount of bariumchloride and EDTA, 90-95 ℃ of processing 1-2 hour of decolouring down, to filter down in 90 ℃ behind the adding diatomite, filtrate is separated out crystallization under the vacuum, centrifugation, filtrate is recycled to the extraction dog-house and does to extract liquid usefulness for the first time, and filter cake carries out vacuum-drying, obtains smart crystalline gallic acid product, drawing the pure back of powder ratio defective product by the raw material tower is 71-72%, accounts for the 75-77% of coarse crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91102322 CN1057255A (en) | 1991-04-10 | 1991-04-10 | Utilize tower to draw powder to produce gallic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91102322 CN1057255A (en) | 1991-04-10 | 1991-04-10 | Utilize tower to draw powder to produce gallic acid |
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| Publication Number | Publication Date |
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| CN1057255A true CN1057255A (en) | 1991-12-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 91102322 Pending CN1057255A (en) | 1991-04-10 | 1991-04-10 | Utilize tower to draw powder to produce gallic acid |
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| CN (1) | CN1057255A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052511C (en) * | 1993-07-08 | 2000-05-17 | 贵州省化工研究院 | Technology for preparation of gallic acid by using enzyme process |
| CN100391931C (en) * | 2006-07-24 | 2008-06-04 | 乐山三江生化科技有限公司 | Direct synthesis process of propyl gallate with Tala powder |
| CN100567446C (en) * | 2007-07-26 | 2009-12-09 | 中国林业科学研究院资源昆虫研究所 | The preparation method of drilling diluter of TARA sulfonated tannin |
| CN106349047A (en) * | 2016-08-02 | 2017-01-25 | 遵义市倍缘化工有限责任公司 | Method using organic strong base to prepare gallic acid under normal pressure |
| CN107954862A (en) * | 2017-12-21 | 2018-04-24 | 张家界久瑞生物科技有限公司 | A kind of method that gallic acid is prepared in liquid caustic soda hydrolysis using defoamer |
| CN108003012A (en) * | 2017-12-21 | 2018-05-08 | 张家界久瑞生物科技有限公司 | A kind of tower draws the method that powder prepares gallic acid |
| CN110922327A (en) * | 2019-12-09 | 2020-03-27 | 邱洪 | Gallic acid acidizing device |
| WO2023051745A1 (en) * | 2021-09-30 | 2023-04-06 | 上海百斯杰生物工程有限公司 | Method for producing gallic acid |
-
1991
- 1991-04-10 CN CN 91102322 patent/CN1057255A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052511C (en) * | 1993-07-08 | 2000-05-17 | 贵州省化工研究院 | Technology for preparation of gallic acid by using enzyme process |
| CN100391931C (en) * | 2006-07-24 | 2008-06-04 | 乐山三江生化科技有限公司 | Direct synthesis process of propyl gallate with Tala powder |
| CN100567446C (en) * | 2007-07-26 | 2009-12-09 | 中国林业科学研究院资源昆虫研究所 | The preparation method of drilling diluter of TARA sulfonated tannin |
| CN106349047A (en) * | 2016-08-02 | 2017-01-25 | 遵义市倍缘化工有限责任公司 | Method using organic strong base to prepare gallic acid under normal pressure |
| CN107954862A (en) * | 2017-12-21 | 2018-04-24 | 张家界久瑞生物科技有限公司 | A kind of method that gallic acid is prepared in liquid caustic soda hydrolysis using defoamer |
| CN108003012A (en) * | 2017-12-21 | 2018-05-08 | 张家界久瑞生物科技有限公司 | A kind of tower draws the method that powder prepares gallic acid |
| CN107954862B (en) * | 2017-12-21 | 2021-01-29 | 张家界久瑞生物科技有限公司 | Method for preparing gallic acid by adopting defoaming agent in liquid caustic soda hydrolysis |
| CN110922327A (en) * | 2019-12-09 | 2020-03-27 | 邱洪 | Gallic acid acidizing device |
| WO2023051745A1 (en) * | 2021-09-30 | 2023-04-06 | 上海百斯杰生物工程有限公司 | Method for producing gallic acid |
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