CN1453262A - Production process of pyrogallic acid - Google Patents
Production process of pyrogallic acid Download PDFInfo
- Publication number
- CN1453262A CN1453262A CN 03117943 CN03117943A CN1453262A CN 1453262 A CN1453262 A CN 1453262A CN 03117943 CN03117943 CN 03117943 CN 03117943 A CN03117943 A CN 03117943A CN 1453262 A CN1453262 A CN 1453262A
- Authority
- CN
- China
- Prior art keywords
- decarboxylation
- narrow
- pyrogallol
- drainage
- earthen jar
- 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
- WQGWDDDVZFFDIG-UHFFFAOYSA-N pyrogallol Chemical compound OC1=CC=CC(O)=C1O WQGWDDDVZFFDIG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000006114 decarboxylation reaction Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 7
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 16
- 229940079877 pyrogallol Drugs 0.000 claims description 16
- 229940074391 gallic acid Drugs 0.000 claims description 8
- 235000004515 gallic acid Nutrition 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 21
- 238000005516 engineering process Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 7
- 239000002893 slag Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 150000005207 1,3-dihydroxybenzenes Chemical class 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 1
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The production process of pyrogallic acid includes the steps of: dewatering material, decarboxylation, conducting with CO2 gas, once discharge, crystallization, once grading, etc. The production process has no supplementary material and solvent added, low power consumption, low production cost, simple technological steps, and high product quality and yield.
Description
Technical field
The present invention relates to a kind of production method of pyrogallol.
Background technology
Produce the method for pyrogallol at present, remove and use pimelinketone, hexalin, Resorcinols etc. are outside the chemical synthesis of raw material, also having with the gallic acid is the vacuum decarboxylation method of raw material, normal pressure decarboxylation method, pressurization decarboxylation method, microorganism decarboxylation method etc., in recent years also having report to adopt tower to draw powder is the single stage method that raw material directly prepares pyrogallol, chemical synthesis wherein, pressurization synthesis method and microorganism synthesis method still do not have the report of suitability for industrialized production, and real industrialized production method is only for being the vacuum decarboxylation method and the normal pressure decarboxylation method of raw material with the gallic acid, and comparatively general and ripe with vacuum decarboxylation method, but mainly there is following shortcoming in vacuum decarboxylation method:
1, decarboxylation is heated to be the single bottom surface heating of decarboxylation narrow-necked earthen jar, the temperature height, general above 250 ℃, the material heating is irregular, and waste energy, especially because of the heating of bottom surface only, decarboxylation narrow-necked earthen jar internal upper part temperature is lower, make the distillation gas that has just sublimed up into top after the decarboxylation do not shift to as yet the crystallization narrow-necked earthen jar again part recovery rate is reduced.
2, the decarboxylation distillation is only adopted the little air drainage once in a while or is not carried out the gas drainage, does not more adopt CO
2Drainage can not quicken and stablize distillation gas and shift to the speed of crystallization narrow-necked earthen jar, thereby the gas that can not guarantee to distil is not only pure but also shift to the crystallization narrow-necked earthen jar timely, and makes recovery rate low.Because of O is arranged in the air
2And SO
2Deng impurity, use air conduction, not only dangerous but also influence the crystalline product quality.
3, adopt two to walk out of material, the special slag that burns of second step causes the production cycle long and latter temperature is very high had both wasted the energy and time, also often because of the temperature height makes decarboxylation narrow-necked earthen jar base plate because of the high temperature creep tension set, has influenced service life of equipment and functional quality.
Also there is the coking flavescence in the pyrogallol of aforesaid method production, and the higher shortcoming of metal ion content such as iron, sodium in the pyrogallol.
Summary of the invention
The object of the present invention is to provide and do not add auxiliary material in a kind of production process, do not use solvent, saved the energy, reduced cost, simplified technology, improved the production method of the pyrogallol of quality product and output.
The inventor studies for a long period of time to the production method of pyrogallol, through repetition test, physico-chemical property according to pyrogallol, and the optimization decarboxylation sublimation condition of gallic acid, to traditional decarboxylation method used adoption of innovation of pyrogallol " low temperature " balanced heating new technology (the decarboxylation narrow-necked earthen jar single bottom surface heating that is about in the traditional method changes the balanced heating technique of decarboxylation narrow-necked earthen jar interlayer " low temperature " into, and maximum operating temperature is no more than 180 ℃); CO
2Drainage technology (is about to the CO that produces in the decarboxylation procedure
2Gas is filtered oil removing, separate relevant purifying treatment such as dewater after, the drainage technology of decarboxylation narrow-necked earthen jar is gone in the part drainage); One walks out of the not slag roasting novel technique of material (be about to two and walk out of material and change into and walk out of material, do not carry out for two steps slag roasting one specially and walk out of material and do not burn the slag technology), has finished the present invention.
The production method of a kind of pyrogallol of the present invention may further comprise the steps:
(1) the raw material gallic acid is dewatered to 90% weight by delivering to drying room in batches;
(2) deliver in the decarboxylation narrow-necked earthen jar and heat, temperature is controlled in the 110-170 ℃ of scope, opens vacuum system
Unite to 0.06-0.08Mpa and begin material distillation;
(3) CO that decarboxylic reaction is produced
2Gas in time returns the decarboxylation narrow-necked earthen jar by gas treatment equipment cleaning back drainage and carries out drainage;
(4) through a back discharging about 16hr;
(5) crystallization, scalping, pack finished product.
The production method of a kind of pyrogallol of the present invention, wherein temperature is controlled in the 110-170 ℃ of scope.
Key problem in technology of the present invention is the physico-chemical property according to pyrogallol, and the optimization decarboxylation sublimation condition of gallic acid, and traditional pyrogallol decarboxylation process innovation has been adopted " low temperature " balanced heating new technology; Adopted CO
2Drainage technology; One walks out of the not slag roasting novel technique of material.Not only simplified technology, and because " low temperature " novel process and CO
2The employing of drainage technology has significantly reduced energy consumption, has avoided equipment to be subjected to the high temperature creep tension set simultaneously, has prolonged the work-ing life of equipment.The unit consumption of raw material gallic acid is reduced to about 2.1t/t about by traditional technology 2.5t/t, has reduced production cost, has improved economic benefit.Because the application of " low temperature " novel process, quality product all meets every quality index of reagent, (seeing standard Q/LHX001-2002) also obviously increased product improved whiteness appearance luster, strengthened the competitive capacity of product on market.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The production method of a kind of pyrogallol of the present invention may further comprise the steps:
(1) raw material gallic acid 100Kg is dewatered to 90% weight by delivering to drying room in batches;
(2) deliver in the decarboxylation narrow-necked earthen jar and heat, temperature is controlled in the 110-170 ℃ of scope, opens vacuum system and begins the material distillation to 0.06-0.08Mpa;
(3) CO that decarboxylic reaction is produced
2Gas in time returns the decarboxylation narrow-necked earthen jar by gas treatment equipment cleaning back drainage and carries out drainage;
(4) through a back discharging about 16hr;
(5) crystallization, scalping, pack finished product, output is 47.6%, i.e. 47.6Kg.
Claims (1)
1, a kind of production method of pyrogallol may further comprise the steps:
(1) the raw material gallic acid is dewatered to 90% weight by delivering to drying room in batches;
(2) deliver in the decarboxylation narrow-necked earthen jar and heat, temperature is controlled in the 110-170 ℃ of scope, opens vacuum system and begins the material distillation to 0.06-0.08Mpa;
(3) the CO2 gas that decarboxylic reaction is produced in time cleans the back drainage by gas treatment equipment and returns the decarboxylation narrow-necked earthen jar and carry out drainage;
(4) through a back discharging about 16hr;
(5) crystallization, scalping, pack finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03117943 CN1209338C (en) | 2003-05-23 | 2003-05-23 | Production process of pyrogallic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03117943 CN1209338C (en) | 2003-05-23 | 2003-05-23 | Production process of pyrogallic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1453262A true CN1453262A (en) | 2003-11-05 |
| CN1209338C CN1209338C (en) | 2005-07-06 |
Family
ID=29260211
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03117943 Expired - Fee Related CN1209338C (en) | 2003-05-23 | 2003-05-23 | Production process of pyrogallic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1209338C (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100336791C (en) * | 2005-07-29 | 2007-09-12 | 保廷荣 | Coupling type heating method for preparing pyrogallic acid |
| CN101161628B (en) * | 2007-11-15 | 2010-06-16 | 浙江大学 | Method for simultaneous preparation of gallic acid and pyrogallic acid by non-catalytic hydrolysis of tannin-containing biomass in high-temperature liquid aqueous medium |
| CN101928204A (en) * | 2009-06-18 | 2010-12-29 | 遵义林源医药化工有限责任公司 | Production method of high-purity pyrogallol |
| CN102671411A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Device for recovering pyrogallic acids through electrostatic adsorption by using sublimation method |
| CN102671413A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Multi-point multi-temperature control coking gallic acid sublimation device for sublimation method |
| CN103449977A (en) * | 2013-08-19 | 2013-12-18 | 竹山县天新医药化工有限责任公司 | Pyrogallic acid production method |
| CN106220476A (en) * | 2016-08-02 | 2016-12-14 | 遵义市倍缘化工有限责任公司 | A kind of low pressure catalytic prepares the method for pyrogallic acid |
| CN106621441A (en) * | 2016-11-10 | 2017-05-10 | 遵义林源医药化工有限责任公司 | Sublimation kettle and method for preparing pyrogallic acid by utilizing same |
| CN107445804A (en) * | 2017-08-25 | 2017-12-08 | 贵州自然生物科技有限公司 | A kind of high-purity pyrogallol production method |
| CN109400447A (en) * | 2018-11-13 | 2019-03-01 | 科利生物科技（徐州）有限公司 | The preparation method of pyrogallol |
| CN109534962A (en) * | 2018-12-18 | 2019-03-29 | 湘潭大学 | The method of pyrogallic acid is prepared using organic amine as gallate decarboxylation accelerant |
| CN111517924A (en) * | 2020-04-24 | 2020-08-11 | 遵义市倍缘化工有限责任公司 | Method for producing pyrogallic acid by using tannic acid |
-
2003
- 2003-05-23 CN CN 03117943 patent/CN1209338C/en not_active Expired - Fee Related
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100336791C (en) * | 2005-07-29 | 2007-09-12 | 保廷荣 | Coupling type heating method for preparing pyrogallic acid |
| CN101161628B (en) * | 2007-11-15 | 2010-06-16 | 浙江大学 | Method for simultaneous preparation of gallic acid and pyrogallic acid by non-catalytic hydrolysis of tannin-containing biomass in high-temperature liquid aqueous medium |
| CN101928204A (en) * | 2009-06-18 | 2010-12-29 | 遵义林源医药化工有限责任公司 | Production method of high-purity pyrogallol |
| CN102671411A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Device for recovering pyrogallic acids through electrostatic adsorption by using sublimation method |
| CN102671413A (en) * | 2012-05-16 | 2012-09-19 | 六盘水神驰生物科技有限公司 | Multi-point multi-temperature control coking gallic acid sublimation device for sublimation method |
| CN102671411B (en) * | 2012-05-16 | 2015-01-14 | 六盘水神驰生物科技有限公司 | Device for recovering pyrogallic acids through electrostatic adsorption by using sublimation method |
| CN103449977A (en) * | 2013-08-19 | 2013-12-18 | 竹山县天新医药化工有限责任公司 | Pyrogallic acid production method |
| CN103449977B (en) * | 2013-08-19 | 2015-09-30 | 竹山县天新医药化工有限责任公司 | A kind of production method of pyrogallol |
| CN106220476A (en) * | 2016-08-02 | 2016-12-14 | 遵义市倍缘化工有限责任公司 | A kind of low pressure catalytic prepares the method for pyrogallic acid |
| CN106220476B (en) * | 2016-08-02 | 2018-12-18 | 遵义市倍缘化工有限责任公司 | A kind of method that low pressure catalytic prepares pyrogallic acid |
| CN106621441A (en) * | 2016-11-10 | 2017-05-10 | 遵义林源医药化工有限责任公司 | Sublimation kettle and method for preparing pyrogallic acid by utilizing same |
| CN106621441B (en) * | 2016-11-10 | 2019-01-25 | 遵义林源医药化工有限责任公司 | A method of distillation and prepares pyrogallic acid using it at kettle |
| CN107445804A (en) * | 2017-08-25 | 2017-12-08 | 贵州自然生物科技有限公司 | A kind of high-purity pyrogallol production method |
| CN109400447A (en) * | 2018-11-13 | 2019-03-01 | 科利生物科技（徐州）有限公司 | The preparation method of pyrogallol |
| CN109534962A (en) * | 2018-12-18 | 2019-03-29 | 湘潭大学 | The method of pyrogallic acid is prepared using organic amine as gallate decarboxylation accelerant |
| CN111517924A (en) * | 2020-04-24 | 2020-08-11 | 遵义市倍缘化工有限责任公司 | Method for producing pyrogallic acid by using tannic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1209338C (en) | 2005-07-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1209338C (en) | Production process of pyrogallic acid | |
| CN103113187A (en) | Method for producing ethanol and coproducing ethyl acetate with acetic acid | |
| CN1693190A (en) | Method for mfg. particle active carbon and light coal tar by tar dregs | |
| CN101029148A (en) | Process of reclaimed rubber by improved high-temperature dynamic desulfurization | |
| CN101041418A (en) | Processes and apparatus for gas production by methanol | |
| CN101182079A (en) | Citric acid mother liquor treatment process | |
| CN102553556B (en) | A kind of regeneration method of active carbon of processing ibuprofen decolorization process | |
| CN1027809C (en) | Method for synthesizing chlorinated paraffin | |
| CN107446966A (en) | A kind of preparation method of D pantolactones | |
| CN102260230B (en) | Method for preparing furfural by using two-step hydrolysis of biomass | |
| US20100293839A1 (en) | Process for making bio-oils and fresh water from aquatic biomass | |
| CN102229858B (en) | Method for preparing biodiesel | |
| CN211050940U (en) | Negative pressure control system for rectifying and cutting medium-chain hydrocarbon by negative pressure condensation method | |
| CN100355647C (en) | Lithium metaphosphorate production process | |
| CN1348942A (en) | Molecular sieve adsorbing and dewatering process of producing absolute alcohol | |
| CN101550065B (en) | Energy-saving and water-saving type high-low pressure double-tower process for preparing dimethyl ether by rectifying methanol | |
| CN1931860A (en) | process of extracting separating and purifying artemisinin from sweet wormwood herb | |
| CN1298617C (en) | Sulfur-melting technology by coke oven gas and device therefor | |
| CN211871868U (en) | Device for efficiently preheating and purifying pyroligneous liquor | |
| CN1027379C (en) | Method for separating quinoline insoluble component in coal tar | |
| CN112409304A (en) | Purification method of intermediate in Grignard section of maltol | |
| CN204918433U (en) | Tricapryl trimellitate apparatus for producing | |
| CN1470616A (en) | Coal gas purifying method | |
| CN2846437Y (en) | Metal sodium slag recovery and treating device | |
| CN1250768A (en) | Process for preparing anthracene, phenanthrene and karbazole |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: LUPANSHUI SHENCHI BIOLOGY TECHNOLOGY LTD. Free format text: FORMER OWNER: HUAXIANG CHEMICAL INDUSTRY CO., LTD., LIUPANSHUI Effective date: 20060728 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20060728 Address after: 553004 Guizhou city of Liupanshui province Zhongshan dewu South Road Patentee after: Liupanshui Shenchi Biotechnology Co., Ltd. Address before: 553001 flower fishing cave, Zijin Mountain District, Guizhou City, Liupanshui province (Shuicheng Brewing Factory) Patentee before: Huaxiang Chemical Industry Co., Ltd., Liupanshui |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050706 Termination date: 20130523 |