CN103408608A - Preparation method of tala industrial tannic acid - Google Patents
Preparation method of tala industrial tannic acid Download PDFInfo
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- CN103408608A CN103408608A CN201310397932XA CN201310397932A CN103408608A CN 103408608 A CN103408608 A CN 103408608A CN 201310397932X A CN201310397932X A CN 201310397932XA CN 201310397932 A CN201310397932 A CN 201310397932A CN 103408608 A CN103408608 A CN 103408608A
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Abstract
The invention discloses a preparation method of tala industrial tannic acid. The preparation method comprises the following step of: leaching tala beanpod and/or beanpod hulls by using acidified diatomite, activated clay and active carbon to obtain leaching solution. According to the invention, crushing treatment is not required to be carried out on the tala beanpod and/or the beanpod hulls as raw materials for preparing the tala industrial tannic acid by adopting the method disclosed by the invention, so that the submicron particles formed after crushing are reduced, the difficulty of filtration is reduced, the impurities leached in a leaching process are reduced due to the integrality of the raw materials, and the obtained tala industrial tannic acid is higher in purity; in addition, because the leaching and refining of the tala industrial tannic acid are integrated into a whole, the leaching process also comprises a refining process, and the leaching is also carried out during the refining. The preparation method disclosed by the invention has the characteristics of simple process, short process flow, high efficiency and high operability and can be applied to the large-scale production of the tala industrial tannic acid.
Description
Technical field
The present invention relates to the preparation method that a kind of tower draws industrial tannic acid.
Background technology
Tara tannic acid can be used for the fields such as food, medicine, chemical industry, metallurgy, wherein the consumption maximum be in field of metallurgy as the germanium precipitation agent, have wide market outlook.
With traditional Weibull raw materials for production Turkey-galls, compare, tower draws in raw material gum level higher, and after lixiviate, solid-liquid separation is difficult to carry out, and can't carry out smoothly the production of Tara tannic acid by traditional Chinese gallotanninic acid production method.
Tower draws in raw material Weibull content approximately 47%～55%, tower after drawing beanpod to pulverize in tower draw raw material through lixiviate, filter after prepared Weibull content generally between 60%～67%, and Weibull is during for the heavy germanium of industry, the content general requirement is more than 78%, so the Tara tannic acid that makes of prior art can't meet the process requirements of the heavy germanium of industry.
For the talas of tannic acid prepared acid content is reached more than 78%, the traditional way in this area is to use the means such as freezing sedimentation, organic solvent extraction, resin purification, membrane filtration at present.But the defect that these methods exist is significantly to have improved production cost.
Summary of the invention
The object of the invention is to overcome existing tower and draw the solid-liquid separation difficulty existed in the preparation process of industrial tannic acid, Weibull content is on the low side, the refining high defect of cost, provide a kind of, without tower is drawn beanpod and/or beanpod shell pulverize, simply, efficiently, the cost less investment, easy and simple to handle can obtain the preparation method that the tower that meets the LY/T1642-2005 standard-required draws industrial tannic acid.
For reaching above purpose, the invention provides the preparation method that a kind of tower draws industrial tannic acid, wherein, the method comprises after with acidifying diatomite, atlapulgite and gac, tower being drawn to beanpod and/or the lixiviate of beanpod shell and obtains vat liquor.
Method provided by the present invention does not need to draw beanpod and/or beanpod shell to carry out pulverization process to the tower as raw material, reduced after pulverizing the ultrafine particle formed, reduced the difficulty of filtering, and, due to the integrity of raw material, make the impurity of stripping in leaching process reduce, the purity of the Weibull obtained is higher, in addition, due to the present invention by the lixiviate of Tara tannic acid, refining being integrated in one, leaching process also comprises treating process, when refining also in lixiviate.Have the advantages that technique is simple, flow process is short, efficiency is high, workable, can be applicable to the large-scale production that tower draws industrial tannic acid.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
The invention provides the preparation method that a kind of tower draws industrial tannic acid, wherein, the method comprises after with acidifying diatomite, atlapulgite and gac, tower being drawn to beanpod and/or the lixiviate of beanpod shell and obtains vat liquor.
In method provided by the present invention, it is the fruit that tower draws tree to tie that described tower draws beanpod, comprises beanpod shell and seed, and it is that tower draws the part after beanpod is removed seed that described tower draws the beanpod shell.
In the present invention, can adopt tower to draw beanpod or tower to draw the beanpod shell as raw material, also tower can be drawn beanpod and beanpod shell to mix the acquisition mixing raw material uses as raw material, when using tower to draw the mixing raw material of beanpod and beanpod shell, ratio for the two has no particular limits, and can be ratio arbitrarily.In preferred situation, the raw material used draws the beanpod shell as tower.
In the present invention, described tower draws beanpod through the tower that shatters processing, not draw beanpod for having, and also can draw beanpod for the tower that particle diameter after pulverizing is greater than 1 * 1cm.In order to simplify follow-up filtration step, reduce the impurity of stripping in leaching process, the present invention preferably adopts the complete tower do not reached through shattering processing to draw beanpod.
In the present invention, described tower draws the beanpod shell through the tower that shatters processing, not draw the beanpod shell for having, and also can draw the beanpod shell for the tower that particle diameter after pulverizing is greater than 1 * 1cm.In order to simplify follow-up filtration step, reduce the impurity of stripping in leaching process, the present invention preferably adopts complete not reaching through the tower that shatters processing to draw the beanpod shell.
In method provided by the present invention, for fear of diatomaceous alkalescence, Tara tannic acid is damaged, need to use the diatomite of acidifying to carry out lixiviate to raw material, in the present invention, for the diatomaceous treatment process of acidifying, do not do special restriction, for example can adopt sulfuric acid or hydrochloric acid to carry out acidification to diatomite, under preferable case, described acidifying diatomite is for to carry out the acidification acquisition with the hydrochloric acid soln that concentration is the 0.1-0.5 % by weight to diatomite, the time of acidification is 10-60min, diatomite with respect to 100g, the consumption of hydrochloric acid soln is the 100-500 milliliter.
Method provided by the present invention has no particular limits the kind of the leaching device that completes the lixiviate step, and for example, leaching process can carry out in this area pot for solvent extraction commonly used or lixiviate cylinder.
In method provided by the present invention, the step of described lixiviate comprises:
(1) tower is drawn beanpod and/or beanpod shell mix with pure water and obtain the first mixture;
(2) the first mixture and acidifying diatomite are contacted and stirs 3-5h and obtain the second mixture;
(3) the second mixture is contacted and stirs 30-60min with gac with atlapulgite and obtain the 3rd mixture;
(4) stop stirring the standing 30-60min of the 3rd mixture.
Wherein, in step (1), the method of drawing beanpod and/or beanpod shell to mix with pure water in tower has no particular limits, after tower can being drawn to beanpod and/or beanpod shell and pure water mixing, add in leaching device, also can join in leaching device respectively for tower being drawn to beanpod and/or beanpod shell and water, and draw beanpod and/or beanpod shell and water to add the sequencing of leaching device not require for tower.
In method provided by the present invention, the mode that the first mixture is contacted with acidifying diatomite can be for making acidifying diatomite contact with the first mixture and mixing fully under agitation condition.
In method provided by the present invention, the mode that the second mixture and atlapulgite are contacted with gac can be for making atlapulgite contact with the first mixture with gac and mixing fully under agitation condition, wherein, with before the second mixture contacts, can be first by atlapulgite and gac premix.
Wherein, in step (4), stop stirring and the 3rd mixture carried out to standing purpose and for continuing, draw beanpod and/or beanpod shell to carry out sufficient lixiviate and the mode by natural subsidence makes acid diatomite, atlapulgite and gac fall to the leaching device bottom to tower, forming filtering layer.
In method provided by the present invention, described lixiviate is carried out at the temperature of 30-60 ℃, in order to improve tower in leaching process, draws the extracting effect of beanpod and/or beanpod shell, and preferred, lixiviate is carried out at the temperature of 35-55 ℃.
In method provided by the present invention, tower with respect to 100g draws beanpod and/or beanpod shell, the consumption of described pure water is 1000-3000g, the diatomaceous consumption of acidifying is that the consumption of 1-5g, atlapulgite is that the consumption of 3-6g, gac is 3-6g, in preferred situation, tower with respect to 100g draws beanpod and/or beanpod shell, and the consumption of described pure water is 1500-2500g, and the diatomaceous consumption of acidifying is that the consumption of 1.5-4.5g, atlapulgite is that the consumption of 3.5-5.5g, gac is 3.5-5.5g.
In the present invention, the diatomaceous granular size of described acidifying is the 100-400 order, SiO
2Content>=88.5%, the granular size of described atlapulgite are the 100-300 order, and activity degree is 120-220, and described gac is Powdered Activated Carbon, and iodine number is 700-1000mg/g, methylene blue number 120-180mg/g.
In the present invention, leaching process material used can also comprise that other can adsorb the sorbent material of polysaccharide, protein, gelatin substance except pure water, acid diatomite, atlapulgite and gac, for example polyaluminium sulfate, polymerize aluminum chloride, aluminum oxide.
Method provided by the present invention removes by filter impurity after also being included in standing end of processing, obtains turbidity not higher than the vat liquor of 150NTU.For preferably can adopting the mode of vacuum filtration, the efficiency that improves filtration filters, and when using the filter type of vacuum filtration, the vacuum tightness of suction filtration is-0.03MPa～-0.05MPa.
Method provided by the present invention also comprises that vat liquor is carried out to further post-processing step draws the industrial tannic acid finished product to obtain tower, described post-processing step can comprise vacuum concentration and spraying drying, concrete, the method of described vacuum concentration is for being used rotatory evaporator, at the temperature of 45-65 ℃, be concentrated into solid content to 35-45%, described spray-dired method is for being used small-sized spray drier, at inlet temperature 160-180 ℃, carry out spraying drying under the condition of air outlet temperature 65-80 ℃.
Outward appearance to the Weibull product that obtains after carrying out spraying drying is faint yellow unformed powder, can adopt Weibull analytical test method LY/T1642-2005 to carry out analyzing and testing to the parameters of product, the project of analyzing and testing comprises the Weibull content of sample, weight loss on drying, water insoluble matter content and color.
Below will describe the present invention by embodiment.In following examples:
Pot for solvent extraction is purchased from Shanghai brightness exhibition experimental installation company limited, model HZ-TQG;
Diatomite is purchased from Kowloon, Kunming filtering technique company limited, and the trade mark is clean clear;
Atlapulgite is purchased from District, Xinyang Area, Henan Province city Pingqiao District sunlight wilkinite factory, and the trade mark is sunlight;
Gac is purchased from the blue sea, Changzhou green technology company limited, and the trade mark is the blue sea;
In following examples, utilize Weibull analytical test method LY/T1642-2005 to analyze Weibull content, weight loss on drying, water-insoluble and color in product.
Embodiment 1
Take the 5kg tower and draw the beanpod shell, draw the beanpod shell to drop into the pot for solvent extraction that has added the 90kg pure water in tower, open to stir, add successively 0.15kg to use in advance the diatomite of the hydrochloric acid soln acidifying of 0.2% mass concentration, stirring and leaching 4h, add again 0.23kg atlapulgite and 0.23kg gac, stirring and leaching 45min, stop stirring standing lixiviate 45min again, make the abundant sedimentation of diatomite, atlapulgite and gac, form filtering layer.Stop lixiviate, carry out vacuum filtration, vacuum degree control is at-0.04MPa.The clarification filtered solution obtained after suction filtration, through vacuum concentration, spraying drying, obtains tower and draws industrial tannic acid product 2.6kg.
Product appearance is faint yellow unformed powder, according to the method for standard LY/T1642-2005, detects Weibull content 81.35 % by weight of product, weight loss on drying 6.21 % by weight, water-insoluble 0.52 % by weight, color 0.6 Luo Weibang unit.
Embodiment 2
According to the method identical with embodiment 1, prepare tower and draw industrial tannic acid, different is that the tower used draws raw material to draw beanpod as tower.
Obtain tower and draw industrial tannic acid product 2.21kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.86 % by weight of product, weight loss on drying 6.58 % by weight, water-insoluble 0.56 % by weight, color 0.6 Luo Weibang unit.
Embodiment 3
According to the method identical with embodiment 1, prepare tower and draw industrial tannic acid, different is, the tower used draws raw material to draw beanpod and tower to draw the beanpod shell as tower, and the ratio of the two is 1:1.
Obtain tower and draw industrial tannic acid product 2.3kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.98 % by weight of product, weight loss on drying 5.67 % by weight, water-insoluble 0.53 % by weight, color 0.6 Luo Weibang unit.
Embodiment 4
According to the method identical with embodiment 1, prepare tower and draw industrial tannic acid, different is, the consumption of water is that 75kg, the diatomaceous consumption of acidifying are that the consumption of 0.075kg, atlapulgite is that the consumption of 0.175kg, gac is 0.175kg.
Obtain tower and draw industrial tannic acid product 2.59kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 81.33 % by weight of product, weight loss on drying 5.69 % by weight, water-insoluble 0.55 % by weight, color 0.6 Luo Weibang unit.
Embodiment 5
According to the method identical with embodiment 1, prepare tower and draw industrial tannic acid, different is, the consumption of water is that 125kg, the diatomaceous consumption of acidifying are that the consumption of 0.225kg, atlapulgite is that the consumption of 0.275kg, gac is 0.275kg.
Obtain tower and draw industrial tannic acid product 2.61kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.93 % by weight of product, weight loss on drying 5.6 % by weight, water-insoluble 0.52 % by weight, color 0.6 Luo Weibang unit.
Embodiment 6
According to the method identical with embodiment 1, prepare tower and draw industrial tannic acid, different is, the consumption of water is that 50kg, the diatomaceous consumption of acidifying are that the consumption of 0.05kg, atlapulgite is that the consumption of 0.15kg, gac is 0.15kg.
Obtain tower and draw industrial tannic acid product 2.57kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 78.09 % by weight of product, weight loss on drying 5.77 % by weight, water-insoluble 0.69 % by weight, color 0.8 Luo Weibang unit.
Embodiment 7
According to the method identical with embodiment 1, prepare tower and draw industrial tannic acid, different is, the consumption of water is that 150kg, the diatomaceous consumption of acidifying are that the consumption of 0.25kg, atlapulgite is that the consumption of 0.3kg, gac is 0.3kg.
Obtain tower and draw industrial tannic acid product 2.64kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 79.86 % by weight of product, weight loss on drying 6.1 % by weight, water-insoluble 0.57 % by weight, color 0.7 Luo Weibang unit.
Embodiment 8
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that lixiviate is carried out at the temperature of 30 ℃.
Obtain tower and draw industrial tannic acid product 1.8kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 79.85 % by weight of product, weight loss on drying 4.39 % by weight, water-insoluble 0.56 % by weight, color 0.7 Luo Weibang unit.
Embodiment 9
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that lixiviate is carried out at the temperature of 60 ℃.
Obtain tower and draw industrial tannic acid product 2.6kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 78.93 % by weight of product, weight loss on drying 5.76 % by weight, water-insoluble 0.68 % by weight, color 0.8 Luo Weibang unit.
Embodiment 10
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the vacuum tightness of suction filtration is-0.03MPa.
Obtain tower and draw industrial tannic acid product 2.46kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.02 % by weight of product, weight loss on drying 6.01 % by weight, water-insoluble 0.58 % by weight, color 0.7 Luo Weibang unit.
Embodiment 11
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the vacuum tightness of suction filtration is-0.05MPa.
Obtain tower and draw industrial tannic acid product 2.62kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 78.86 % by weight of product, weight loss on drying 5.67 % by weight, water-insoluble 0.77 % by weight, color 0.7 Luo Weibang unit.
Embodiment 12
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that it is 3h with the mixture of pure water with the time that acidifying diatomite contacts and stirs that tower is drawn to raw material.
Obtain tower and draw industrial tannic acid product 2.61kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.65 % by weight of product, weight loss on drying 5.93 % by weight, water-insoluble 0.59 % by weight, color 0.7 Luo Weibang unit.
Embodiment 13
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that it is 5h with the mixture of pure water with the time that acidifying diatomite contacts and stirs that tower is drawn to raw material.
Obtain tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.01 % by weight of product, weight loss on drying 6.02 % by weight, water-insoluble 0.57 % by weight, color 0.7 Luo Weibang unit.
Embodiment 14
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, the churning time that different is adds after atlapulgite and gac is 30min.
Obtain tower and draw industrial tannic acid product 2.59kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.33 % by weight of product, weight loss on drying 6.32 % by weight, water-insoluble 0.61 % by weight, color 0.8 Luo Weibang unit.
Embodiment 15
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, the churning time that different is adds after atlapulgite and gac is 60min.
Obtain tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.09 % by weight of product, weight loss on drying 6.36 % by weight, water-insoluble 0.61 % by weight, color 0.7 Luo Weibang unit.
Embodiment 16
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the standing time is 30min.
Obtain tower and draw industrial tannic acid product 2.6kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.29 % by weight of product, weight loss on drying 6.87 % by weight, water-insoluble 0.59 % by weight, color 0.7 Luo Weibang unit.
Embodiment 17
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the standing time is 60min.
Obtain tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.11 % by weight of product, weight loss on drying 6.06 % by weight, water-insoluble 0.59 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 1
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the consumption of water is 175kg.
Obtain tower and draw industrial tannic acid product 2.72kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 76.53 % by weight of product, weight loss on drying 6.65 % by weight, water-insoluble 0.57 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 2
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the diatomaceous consumption of acidifying is 0.3kg.
Obtain tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 80.19 % by weight of product, weight loss on drying 5.96 % by weight, water-insoluble 0.9 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 3
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the consumption of atlapulgite is 0.1kg.
Obtain tower and draw industrial tannic acid product 2.6kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 77.01 % by weight of product, weight loss on drying 5.31 % by weight, water-insoluble 0.67 % by weight, color 0.8 Luo Weibang unit.
Comparative Examples 4
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the consumption of gac is 0.33kg.
Obtain tower and draw industrial tannic acid product 2.59kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 76.32 % by weight of product, weight loss on drying 6.1 % by weight, water-insoluble 0.89 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 5
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that lixiviate is carried out at the temperature of 65 ℃.
Obtain tower and draw industrial tannic acid product 2.64kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 77.69 % by weight of product, weight loss on drying 8.39 % by weight, water-insoluble 0.88 % by weight, color 0.8 Luo Weibang unit.
Comparative Examples 6
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the vacuum tightness of suction filtration is-0.06MPa
Obtain tower and draw industrial tannic acid product 2.68kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 77.98 % by weight of product, weight loss on drying 5.4 % by weight, water-insoluble 0.81 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 7
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that it is 2.5h with the mixture of pure water with the time that acidifying diatomite contacts and stirs that tower is drawn to raw material.
Obtain tower and draw industrial tannic acid product 2.4kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 76.88 % by weight of product, weight loss on drying 8.6 % by weight, water-insoluble 0.8 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 8
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, the churning time that different is adds after atlapulgite and gac is 25min.
Obtain tower and draw industrial tannic acid product 2.56kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 76.49 % by weight of product, weight loss on drying 8.4 % by weight, water-insoluble 0.64 % by weight, color 0.7 Luo Weibang unit.
Comparative Examples 9
Adopt the method identical with embodiment 1 to prepare tower and draw industrial tannic acid, different is that the standing time is 25min.
Obtain tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005, Weibull content 76.56 % by weight of product, weight loss on drying 7.65 % by weight, water-insoluble 0.76 % by weight, color 0.7 Luo Weibang unit.
Result by embodiment 1-17 can be found out, utilizes production method provided by the present invention to prepare tower and draws industrial tannic acid can access the product that meets the LY/T1642-2005 standard.And the Weibull content of product is higher than 78.0 % by weight, and weight loss on drying is less than 9.0 % by weight, and water-insoluble is less than 0.8 % by weight, and color is less than 3.0 Luo Weibang units.
By embodiment 1,4 and 5 and the result of embodiment 6 and 7 can find out, when the consumption of the consumption of the diatomaceous consumption of consumption, acidifying of water, atlapulgite, gac is within preferable range of the present invention, the Weibull content of the product obtained is higher, water insoluble matter content is lower, and color is more shallow.
By embodiment 1, can find out with the result of Comparative Examples 1, when amount of water is 175kg, namely soak amount of water when too much, the Weibull content step-down of the product obtained, illustrate and add water to after a certain amount of, the Weibull leaching yield does not continue to raise with the increase of the water yield, now increases the water yield again, only can cause more impurity to leach.
By embodiment 1, can find out with the result of Comparative Examples 2, when acidifying diatomite consumption increases to 0.3kg, Weibull content, water-insoluble and the color of the product obtained are undesirable on the contrary, illustrate in Weibull can by the impurity of acidifying diatomite adsorption be have a certain amount of, after acidifying diatomite adsorbs these impurity fully, increase again diatomaceous amount, do not had positive meaning, be diatomite itself on the contrary with impurity effect the quality of product.
By embodiment 1, can find out with the result of Comparative Examples 3, when the atlapulgite consumption is 0.1kg, the Weibull content of the product obtained is 77.01%, does not reach the requirement more than 78.0%, and the addition deficiency that atlapulgite is described can cause the reduction of Weibull content.
By embodiment 1, can find out with the result of Comparative Examples 4, when activated carbon dosage is 0.33kg, while reaching excess interpolation gac, the quality of the product obtained is not as adding the product of gac gained by optimum usage quantity, illustrate in Weibull to be to have a certain amount ofly by the impurity of charcoal absorption, after gac adsorbs these impurity fully, then increase the amount of gac, do not had positive meaning, be gac itself on the contrary with impurity effect the quality of product.
By embodiment 1, can find out with the result of Comparative Examples 5, when extraction temperature is 65 ℃, Weibull content, water-insoluble and the color of the product obtained all is worse than the product of gained in normal extraction temperature scope, illustrates that the too high quality to Weibull of extraction temperature has caused detrimentally affect.
By embodiment 1, can find out with the result of Comparative Examples 6, when suction filtration vacuum tightness be-during 0.06MPa, the quality of the product of acquisition is not as the product by optimum vacuum tightness suction filtration, when suction filtration was described, vacuum tightness was too high, can cause a certain amount of impurity to wear filter, affect the quality of Weibull.
By embodiment 1, can find out with the result of Comparative Examples 7, when time that the mixture that tower is drawn to raw material and pure water and acidifying diatomite contact and stirs was in the given scope of the present invention, the quality of the Weibull of acquisition was higher.
By embodiment 1, can find out with the result of Comparative Examples 8, when the churning time after interpolation atlapulgite and gac was in the given scope of the present invention, the quality of the Weibull of acquisition was higher.
By embodiment 1, can find out with the result of Comparative Examples 9, when the standing time was in the given scope of the present invention, the quality of the Weibull of acquisition was higher.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, in technical conceive scope of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine for fear of unnecessary repetition by any suitable mode, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out arbitrary combination between various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. a tower draws the preparation method of industrial tannic acid, it is characterized in that, the method comprises after with acidifying diatomite, atlapulgite and gac, tower being drawn to beanpod and/or the lixiviate of beanpod shell and obtains vat liquor.
2. tower according to claim 1 draws the preparation method of industrial tannic acid, and wherein, the step of described lixiviate comprises:
(1) tower is drawn beanpod and/or beanpod shell mix with pure water and obtain the first mixture;
(2) the first mixture and acidifying diatomite are contacted and stirs 3-5h and obtain the second mixture;
(3) the second mixture is contacted and stirs 30-60min with gac with atlapulgite and obtain the 3rd mixture;
(4) stop stirring the standing 30-60min of the 3rd mixture.
3. tower according to claim 1 and 2 draws the preparation method of industrial tannic acid, wherein, tower with respect to 100g draws beanpod and/or beanpod shell, and the consumption of described pure water is 1000-3000g, and the diatomaceous consumption of acidifying is that the consumption of 1-5g, atlapulgite is that the consumption of 3-6g, gac is 3-6g.
4. tower according to claim 3 draws the preparation method of industrial tannic acid, wherein, tower with respect to 100g draws beanpod and/or beanpod shell, the consumption of described pure water is 1500-2500g, and the diatomaceous consumption of acidifying is that the consumption of 1.5-4.5g, atlapulgite is that the consumption of 3.5-5.5g, gac is 3.5-5.5g.
5. tower according to claim 1 draws the preparation method of industrial tannic acid, and wherein, it is the fruit that tower draws tree to tie that described tower draws beanpod, comprises beanpod shell and seed, and it is that tower draws the part after beanpod is removed seed that described tower draws the beanpod shell.
6. prepare according to claim 1 or 5 the method that tower draws industrial tannic acid, wherein, it is that the complete tower that does not draw beanpod or be greater than 1 * 1cm for particle diameter after pulverizing through the tower of pulverization process draws beanpod that described tower draws beanpod;
Wherein, to draw the beanpod shell be that the complete tower that does not draw the beanpod shell or be greater than 1 * 1cm for particle diameter after pulverizing through the tower of pulverization process draws the beanpod shell to described tower.
7. according to the described tower of any one in claim 1,2 and 4, draw the preparation method of industrial tannic acid, wherein, described acidifying diatomite is for to carry out the acidification acquisition with the hydrochloric acid soln that concentration is the 0.1-0.5 % by weight to diatomite, the time of acidification is 10-60min, with respect to the diatomite of 100g, the consumption of hydrochloric acid soln is the 100-500 milliliter.
8. according to claim 1,2,4 and 5 described towers, draw the preparation method of industrial tannic acid, wherein, described lixiviate is carried out at the temperature of 30-60 ℃.
9. tower according to claim 2 draws the preparation method of industrial tannic acid, and wherein, the method also is included in the standing 30-60min final vacuum of the 3rd mixture suction filtration is obtained to vat liquor, and the vacuum tightness of suction filtration is-0.03MPa～-0.05MPa.
10. tower according to claim 1 draws the preparation method of industrial tannic acid, and wherein, the method also comprises that the filtered solution that vacuum filtration is obtained concentrates and be dry.
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Cited By (1)
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| CN107373664A (en) * | 2017-07-18 | 2017-11-24 | 杏辉天力（杭州）药业有限公司 | A kind of composition with anti-PM2.5 particulate matters effect |
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