CN106317134A - Method for preparing glucose and gallic acid by hydrolyzing tannin extract through hydro-thermal method - Google Patents
Method for preparing glucose and gallic acid by hydrolyzing tannin extract through hydro-thermal method Download PDFInfo
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- CN106317134A CN106317134A CN201610700987.7A CN201610700987A CN106317134A CN 106317134 A CN106317134 A CN 106317134A CN 201610700987 A CN201610700987 A CN 201610700987A CN 106317134 A CN106317134 A CN 106317134A
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- gallic acid
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- glucose
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- tannic extract
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/02—Monosaccharides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for preparing glucose and gallic acid by hydrolyzing a tannin extract through a hydro-thermal method. The method comprises the following steps: (1) hydrolyzing the tannin extract for 0.5-2.0h in a high-temperature autoclave under the condition that the pressure is 0.1-2.8MPa and the temperature is 120-240 DEG C, and performing filtration or centrifugation to obtain a hydrolysate solution; (2) neutralizing the hydrolysate by adopting clear limewater to generate a deposit, and performing filtration or centrifugation to obtain a solution and a deposit; (3) performing concentration and spray drying on the solution to obtain the glucose; and (4) acidifying the deposit by adopting a dilute sulfuric acid solution, then adjusting the pH value of the acidified solution to be 4.0-6.0 by using CaCO3 or clear limewater, performing filtration or centrifugation to obtain a solution, and performing concentration and spray drying to obtain the gallic acid. The method disclosed by the invention is implemented by taking water as a solvent under a high-temperature and high-pressure condition, and is environmentally friendly and efficient, the obtained glucose and gallic acid have relatively high economic values, and the added value of the tannin extract can be effectively improved.
Description
Technical field
The present invention relates to the method that chemicals prepared by a kind of hydro-thermal method hydrolysis tannic extract, particularly relate to a kind of hydro-thermal method hydrolysis
The method of glucose and gallic acid prepared by tannic extract, belongs to field of chemical engineering.
Background technology
Tannic extract is a kind of important tanning agent, and mainly in leather industry, tanning uses.In addition, also serve as beneficiation inhibitor,
Water treating agent for boilers, drilling mud diluent, metal surface corrosion inhibitor and adhesive.It is by the plant material warp rich in tannin
The chemical products that hot water extraction, concentration and drying and other steps processing prepare.The main component of tannic extract is tannin, according to its structure
Difference, can be divided into Hydrolysable Tannins and condensed tannin by tannin, and wherein Hydrolysable Tannins refers to be derived by gallic acid or gallic acid
The ester that formed of phenol carboxylic acid and polyhydric alcohol (such as glucose), be widely present in acorn cup, change in Oleum Linderae and Galla Chinensis.In recent years,
In order to open up tannic extract application new way and improve tannic extract higher value application, tannic extract is prepared for by research worker through chemical modification
Some high added value materials, and disclose its technology of preparing patent, as utilized tannic extract to prepare phenol formaldehyde foam
(CN201210575450.4), adhesive (CN95103379.4) and the additive (CN01130562.2) of adhesive, these
Bright patent is all based on that tannic extract polyhydric phenols is structurally-modified prepares its macromolecular material, and utilizes tannic extract to prepare the patent of chemicals relatively
Few.
Hydro-thermal method refers in the pressure vessel sealed, and with water as solvent, the chemistry carried out under conditions of High Temperature High Pressure is anti-
Should.This technology has been widely used in the chemical processes such as hydrolysis, oxidoreduction, crystalline deposit.According to hydro-thermal reaction
The difference of process condition, can be classified as subcritical and supercritical reaction, wherein subcritical reaction temperature 100～240 DEG C it
Between, being suitable to industrialized production, and supercritical reaction temperature is up to thousands of degree, pressure is up to 0.3Gpa, severe reaction conditions.And go
The most traditional tannic extract method for hydrolysis is to use dilute sulfuric acid or dilute hydrochloric acid process tannic extract, pollution environment, and to equipment corrosion relatively
Greatly, the present invention is contemplated to solve environmental pollution and the equipment corrosion problem that above-mentioned acid hydrolysis causes.At present, application hydro-thermal is had no
Method hydrolysis tannic extract prepares glucose and the Patents of gallic acid and research thereof.
This patent uses hydro-thermal method hydrolysis acorn cup, change Oleum Linderae and Galla Chinensis tannic extract to prepare glucose and gallic acid, and it is former
Reason is that water forms H under high-temperature and high-pressure conditions+, to gallic acid in hydrolysable tannins in this tannin extracts and the ester of glucose formation
Key is hydrolyzed, and then prepares glucose and gallic acid.Glucose has extensive and important in medicine food field
Purposes, gallic acid is a kind of important industrial chemicals, also referred to as gallic acid or acid, and chemical name is 3,4,5-trihydroxies
Benzoic acid, has a wide range of applications at food medicine and biological chemical field.At present, on market tannic extract price be 10000 yuan/
Ton, and industrial glucose price is 72000 yuan/ton, and gallic acid price is 70000 yuan/ton, it can be seen that, this patent with
Tannic extract is raw material, uses hydro-thermal method hydrolysis tannic extract to prepare glucose and the gallic acid of high added value, can be effectively improved tannic extract
Higher value application, has huge potential age deduction.
Summary of the invention
The invention aims to environmental pollution and the equipment corrosion problem overcoming acid hydrolysis tannic extract to cause, it is provided that a kind of
The method that hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, this technology belongs to field of chemical engineering.
The purpose of the present invention is achieved through the following technical solutions:
The method that a kind of hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, comprises the following steps:
(1) mass volume ratio of tannic extract and water is 1:10～1:25, in high-temperature high-pressure reaction kettle pressure be 0.1～
2.8MPa, under the conditions of temperature is 120～240 DEG C, stirring reacts 0.5～2.0h, and reactant liquor is cooled to room temperature, the list of described quality
Position is kg, and the unit of described volume is L；
(2) by step (1) described reacting liquid filtering or centrifugal；
(3) step (2) described filtrate or centrifugal liquid are clarified lime water to neutralize, generate precipitation, filter or centrifugal,
To solution and precipitation；
(4) step (3) described solution evaporation is concentrated into 30～40%；
(5) step (4) described concentrated solution is spray-dried, obtains glucose；
(6) step (3) described precipitation dilution heat of sulfuric acid is acidified, then uses CaCO3Or clarification lime water regulation acidifying is molten
Liquid pH is 4.0～6.0, filters or centrifugal；
(7) by step (6) described filtrate or centrifugal liquid evaporation and concentration to 30～40%；
(8) step (7) described concentrated solution is spray-dried, obtains gallic acid.
For realizing the object of the invention further, the tannic extract described in step (1) is acorn cup, changes in Oleum Linderae and Galla Chinensis tannic extract and appoint
What is a kind of.
Step (2), step (3) and step (6) described centrifugal rotational speed are 1000～5000rpm/min, centrifugation time be 5～
20min。
Step (4) and step (7) described evaporation and concentration be system of three-effect downstream evaporator concentrate, one effect pressure be 0.05～
1.0MPa, temperature 100～110 DEG C, concentration is 5～8%, two effect pressure be 0MPa, temperature 100～110 DEG C, concentration be 20～
25%, triple effect pressure-0.004～-0.005MPa, temperature is 100～110 DEG C, and concentration is 30～40%.
Step (6) described dilution heat of sulfuric acid concentration is 0.1～1.0M.
Spray drying described in step (5) and step (8) is pressure spray dryer, centrifugal spray drying, air-flowing type spraying
Any one in Gan Zaoing.
Beneficial effect
Have not yet to see any employing hydro-thermal method hydrolysis tannic extract and prepare glucose and gallic acid technical patent and research public affairs
Open, the present invention under high-temperature and high-pressure conditions using water as solvent, environmental protection, efficiently, and the glucose and the gallic acid that obtain have
Higher economic worth.
Accompanying drawing explanation
Accompanying drawing 1 prepares glucose and gallic acid process flow diagram for hydro-thermal method hydrolysis tannic extract.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, invention is described in further detail, but embodiments of the present invention are not limited to
This.
Embodiment 1
The method that the present embodiment hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, comprises the following steps:
(1) weigh valonea extract 1kg, join in 10L water, stirring reaction under the conditions of temperature 120 DEG C, pressure 0.1Mpa
0.5h, reactant liquor is cooled to room temperature；
(2) by step (1) described reacting liquid filtering；
(3) step (2) described filtrate clarification lime water is neutralized, generate precipitation, filter, obtain solution and precipitation；
(4) step (3) described filtrate employing system of three-effect downstream evaporator is concentrated into 30%；
(5) step (4) described concentrated solution employing centrifugal spray drying is i.e. obtained glucose, yield 10%, purity 75%；
(6) step (3) described precipitation 0.1M dilution heat of sulfuric acid is acidified, then uses CaCO3Regulation souring soln pH is
4.0, filter；
(7) step (6) described filtrate employing system of three-effect downstream evaporator is concentrated into 30%；
(8) step (7) described concentrated solution is used pressure spray dryer, obtain gallic acid, yield 18%, purity
85%.
Embodiment 2
The method that the present embodiment hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, comprises the following steps:
(1) weighing Oleum Linderae tannic extract 1kg, joins in 25L water, and under the conditions of temperature 240 DEG C, pressure 2.8Mpa, stirring is anti-
2.0h, reactant liquor is answered to be cooled to room temperature；
(2) by step (1) described reactant liquor centrifugal 20min under rotating speed 1000rpm/min；
(3) described for step (2) centrifugal liquid clarification lime water of crossing is neutralized, generate precipitation, under rotating speed 1000rpm/min
Centrifugal 20min, obtains solution and precipitation；
(4) step (3) described centrifugal liquid employing system of three-effect downstream evaporator is concentrated into 40%；
(5) step (4) described concentrated solution employing pressure spray dryer is i.e. obtained glucose, yield 8%, purity 70%；
(6) step (3) described precipitation 1.0M dilution heat of sulfuric acid is acidified, then regulates souring soln pH with clarification lime water
It is 6.0, centrifugal 20min under rotating speed 1000rpm/min；
(7) step (6) described filtrate employing system of three-effect downstream evaporator is concentrated into 40%；
(8) step (7) described concentrated solution is used pneumatic spray drying, obtain gallic acid, yield 20%, purity
90%.
Embodiment 3
The method that the present embodiment hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, comprises the following steps:
(1) weighing Galla Chinensis tannic extract 1kg, join in 20L water, under the conditions of temperature 140 DEG C, pressure 0.5Mpa, stirring is anti-
1.0h, reactant liquor is answered to be cooled to room temperature；
(2) by step (1) described reactant liquor centrifugal 5min under rotating speed 5000rpm/min；
(3) described for step (2) centrifugal liquid clarification lime water of crossing is neutralized, generate precipitation, under rotating speed 5000rpm/min
Centrifugal 5min, obtains solution and precipitation；
(4) step (3) described centrifugal liquid employing system of three-effect downstream evaporator is concentrated into 32%；
(5) step (4) described concentrated solution employing pneumatic spray drying is i.e. obtained glucose, yield 12%, purity 80%；
(6) step (3) described precipitation 0.5M dilution heat of sulfuric acid is acidified, then uses CaCO3Regulation souring soln pH is
5.0, centrifugal 5min under rotating speed 5000rpm/min；
(7) step (6) described centrifugal liquid employing system of three-effect downstream evaporator is concentrated into 33%；
(8) step (7) described concentrated solution is used centrifugal spray drying, obtain gallic acid, yield 22%, purity
92%.
Embodiment 4
The method that the present embodiment hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, comprises the following steps:
(1) weigh valonea extract 1kg, join in 15L water, stirring reaction under the conditions of temperature 160 DEG C, pressure 1.0Mpa
1.5h, reactant liquor is cooled to room temperature；
(2) by step (1) described reacting liquid filtering；
(3) by step (2) described filtrate clarification lime water neutralize, generate precipitation, under rotating speed 3000rpm/min from
Heart 10min, obtains solution and precipitation；
(4) step (3) described centrifugal liquid employing system of three-effect downstream evaporator is concentrated into 36%；
(5) step (4) described concentrated solution employing centrifugal spray drying is i.e. obtained glucose, yield 15%, purity 85%；
(6) step (3) described precipitation 0.3M dilution heat of sulfuric acid is acidified, then regulates souring soln with clarification lime water
PH is 5.5, filters；
(7) step (6) described filtrate employing system of three-effect downstream evaporator is concentrated into 34%；
(8) step (7) described concentrated solution is used centrifugal spray drying, obtain gallic acid, yield 24%, purity
93%.
Embodiment 5
The method that the present embodiment hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, comprises the following steps:
(1) weighing Galla Chinensis tannic extract 1kg, join in 18L water, under the conditions of temperature 200 DEG C, pressure 1.5Mpa, stirring is anti-
1.2h, reactant liquor is answered to be cooled to room temperature；
(2) by step (1) described reactant liquor centrifugal 15min under rotating speed 2500rpm/min；
(3) step (2) described centrifugal liquid clarification lime water is neutralized, generate precipitation, filter, obtain solution and precipitation；
(4) step (3) described filtrate employing system of three-effect downstream evaporator is concentrated into 38%；
(5) step (4) described concentrated solution employing pneumatic spray drying is i.e. obtained glucose, yield 14%, purity 87%；
(6) step (3) described precipitation 0.8M dilution heat of sulfuric acid is acidified, then uses CaCO3Regulation souring soln pH is
4.5, centrifugal 12min under rotating speed 1500rpm/min；
(7) step (6) described filtrate employing system of three-effect downstream evaporator is concentrated into 37%；
(8) step (7) described concentrated solution is used pressure spray dryer, obtain gallic acid, yield 25%, purity
94%.
Finally it is noted that the foregoing is only the preferred embodiments of the present invention, it is not limited to the present invention,
Although being described in detail the present invention with reference to previous embodiment, for a person skilled in the art, it still may be used
So that the technical scheme described in foregoing embodiments to be modified, or wherein portion of techniques feature is carried out equivalent,
All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the present invention's
Within protection domain.
Claims (6)
1. the method that a hydro-thermal method hydrolysis tannic extract prepares glucose and gallic acid, it is characterised in that comprise the following steps:
(1) tannic extract is 1:10～1:25 with the mass volume ratio of water, and in high-temperature high-pressure reaction kettle, pressure is 0.1～2.8MPa,
Under the conditions of temperature is 120～240 DEG C, stirring reacts 0.5～2.0h, and reactant liquor is cooled to room temperature, and the unit of described quality is kg,
The unit of described volume is L；
(2) by step (1) described reacting liquid filtering or centrifugal；
(3) step (2) described filtrate or centrifugal liquid are clarified lime water to neutralize, generate precipitation, filter or centrifugal, obtain molten
Liquid and precipitation；
(4) step (3) described solution evaporation is concentrated into 30～40%；
(5) step (4) described concentrated solution is spray-dried, obtains glucose；
(6) step (3) described precipitation dilution heat of sulfuric acid is acidified, then uses CaCO3Or clarification lime water regulation souring soln pH is
4.0～6.0, filter or centrifugal；
(7) by step (6) described filtrate or centrifugal liquid evaporation and concentration to 30～40%；
(8) step (7) described concentrated solution is spray-dried, obtains gallic acid.
The method that hydro-thermal method the most according to claim 1 hydrolysis tannic extract prepares glucose and gallic acid, it is characterised in that
Tannic extract described in step (1) is acorn cup, changes any one of Oleum Linderae and Galla Chinensis tannic extract.
The method that hydro-thermal method the most according to claim 1 hydrolysis tannic extract prepares glucose and gallic acid, it is characterised in that
Step (2), step (3) and step (6) described centrifugal rotational speed are 1000～5000rpm/min, and centrifugation time is 5～20min.
The method that hydro-thermal method the most according to claim 1 hydrolysis tannic extract prepares glucose and gallic acid, it is characterised in that
Step (4) and step (7) described evaporation and concentration are that system of three-effect downstream evaporator concentrates, and an effect pressure is 0.05～1.0MPa, temperature 100
～110 DEG C, concentration is 5～8%, and two effect pressure are 0MPa, temperature 100～110 DEG C, and concentration is 20～25%, triple effect pressure-
0.004～-0.005MPa, temperature is 100～110 DEG C, and concentration is 30～40%.
The method that hydro-thermal method the most according to claim 1 hydrolysis tannic extract prepares glucose and gallic acid, it is characterised in that
Step (6) described dilution heat of sulfuric acid concentration is 0.1～1.0M.
The method that hydro-thermal method the most according to claim 1 hydrolysis tannic extract prepares glucose and gallic acid, it is characterised in that
Being spray-dried as in pressure spray dryer, centrifugal spray drying, pneumatic spray drying described in step (5) and step (8)
Any one.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111454143A (en) * | 2020-05-13 | 2020-07-28 | 遵义市倍缘化工有限责任公司 | Method for preparing gallic acid by hydrolyzing sulfuric acid capable of utilizing by-product |
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| 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 |
| CN101161628A (en) * | 2007-11-15 | 2008-04-16 | 浙江大学 | Method for preparing gallic acid and pyrogallic acid synchronously by non-catalyzed hydrolysis of tannin-containing biomass in high-temperature liquid water medium |
| CN102977548A (en) * | 2012-12-27 | 2013-03-20 | 北京莱恩斯高新技术有限公司 | Vegetable tannin extract modified phenol formaldehyde foam and preparation method thereof |
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| CN1117986A (en) * | 1995-05-07 | 1996-03-06 | 柴万知 | Method for producing tannin-extract adhesive |
| CN1422928A (en) * | 2001-12-02 | 2003-06-11 | 杨文章 | Additive of applying condensed tannin extracts as adhesive for thermosetting wood |
| 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 |
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| CN111454143A (en) * | 2020-05-13 | 2020-07-28 | 遵义市倍缘化工有限责任公司 | Method for preparing gallic acid by hydrolyzing sulfuric acid capable of utilizing by-product |
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