CN103408608B - A kind of tower draws the preparation method of industrial tannic acid - Google Patents
A kind of tower draws the preparation method of industrial tannic acid Download PDFInfo
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- CN103408608B CN103408608B CN201310397932.XA CN201310397932A CN103408608B CN 103408608 B CN103408608 B CN 103408608B CN 201310397932 A CN201310397932 A CN 201310397932A CN 103408608 B CN103408608 B CN 103408608B
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Abstract
The invention discloses a kind of tower and draw the preparation method of industrial tannic acid, wherein, the method obtains lixiviating solution after including extracting Tara seeds pod and/or soybean pod shell with acidifying kieselguhr, active hargil and activated carbon.Use method provided by the present invention to prepare tower to draw industrial tannic acid to need not Tara seeds pod and/or the soybean pod shell as raw material to carry out pulverization process, the ultramicro powder formed after decreasing pulverizing, reduce the difficulty of filtration, and, due to the integrity of raw material, the impurity making dissolution in leaching process reduces, the purity of tannic acid obtained is higher, further, since the present invention by the extraction of Tara tannic acid, refined be integrated in one, leaching process also includes subtractive process, also in extraction time refined.Have the advantages that technique is simple, flow process is short, efficiency is high, workable, can be applicable to tower and draw the large-scale production of industrial tannic acid.
Description
Technical field
This utility model relates to a kind of tower and draws the preparation method of industrial tannic acid.
Background technology
Tara tannic acid can be used for the fields such as food, medicine, chemical industry, metallurgy, and wherein consumption is maximum
Be as germanium precipitant in field of metallurgy, there is wide market prospect.
Comparing with traditional tannic acid raw materials for production Galla Chinensis, tower draws gum level in raw material higher,
After extraction, solid-liquid separation is difficult to, and cannot enter smoothly by traditional Chinese gallotanninic acid production method
The production of row Tara tannic acid.
Tower draws tannic acid content about 47%～55% in raw material, and the tower after being pulverized by Tara seeds pod draws former
Material tannic acid content obtained by after extraction, filtration is typically between 60%～67%, and tannin
During acid germanium heavy for industry, content typically requires more than 78%, the tower that therefore prior art prepares
Draw tannic acid cannot meet the process requirements of the heavy germanium of industry.
In order to make the talas of tannic acid acid content prepared reach more than 78%, current this area tradition
Way be to use the means such as freezing sedimentation, organic solvent extraction, resin purification, membrane filtration.But
The defect that these methods exist is that the cost of production is greatly improved.
Summary of the invention
It is an object of the invention to overcome existing tower to draw present in the preparation process of industrial tannic acid
Solid-liquid separation difficulty, tannic acid content is on the low side, the defect that refined cost is high, it is provided that a kind of, it is not necessary to
Tara seeds pod and/or soybean pod shell are pulverized, simply, efficiently, cost less investment, easy and simple to handle
Be obtained in that meeting the tower of LY/T1642-2005 standard-required draws the preparation side of industrial tannic acid
Method.
For reaching object above, the invention provides a kind of tower and draw the preparation method of industrial tannic acid,
Wherein, the method includes with acidifying kieselguhr, active hargil and activated carbon Tara seeds pod and/or bean
Lixiviating solution is obtained after the extraction of pod shell.
Method provided by the present invention need not enter Tara seeds pod and/or the soybean pod shell as raw material
Row pulverization process, the ultramicro powder formed after decreasing pulverizing, reduce the difficulty of filtration, and,
Integrity due to raw material so that the impurity of dissolution in leaching process reduces, it is thus achieved that tannic acid
Purity is higher, further, since the present invention by the extraction of Tara tannic acid, refined be integrated in one, leaching
The process that carries also includes subtractive process, also in extraction time refined.Have that technique is simple, flow process is short, effect
The feature that rate is high, workable, can be applicable to tower and draws the large-scale production of industrial tannic acid.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that this place is retouched
The detailed description of the invention stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides a kind of tower and draw the preparation method of industrial tannic acid, wherein, the method includes with acid
SiClx diatomaceous earth, active hargil and activated carbon obtain lixiviating solution after extracting Tara seeds pod and/or soybean pod shell.
In method provided by the present invention, the fruit that described Tara seeds pod draws tree to be tied by tower, including bean
Pod shell and seed, described Tara seeds pod shell is the part after Tara seeds pod removes seed.
In the present invention, Tara seeds pod or Tara seeds pod shell can be used as raw material, it is also possible to by tower
Draw soybean pod and the mixing of soybean pod shell to obtain mixing raw material to use as raw material, when using Tara seeds pod and soybean pod shell
Mixing raw material time, the ratio for the two has no particular limits, and can be arbitrary ratio.Preferably
In the case of, the raw material used is Tara seeds pod shell.
In the present invention, described Tara seeds pod can be the Tara seeds pod not processed through smashing, it is possible to
Think the particle diameter Tara seeds pod more than 1 × 1cm after pulverizing.Reduce to simplify follow-up filtration step
The impurity of dissolution in leaching process, present invention preferably employs the complete tower not having and processing through smashing and draws
Soybean pod.
In the present invention, described Tara seeds pod shell can be the Tara seeds pod shell not processed through smashing,
It can also be the particle diameter Tara seeds pod shell more than 1 × 1cm after pulverizing.In order to simplify follow-up filtration step
Die-off the impurity of dissolution in few leaching process, present invention preferably employs complete not having and process through smashing
Tara seeds pod shell.
In method provided by the present invention, in order to avoid Tara tannic acid is caused brokenly by diatomaceous alkalescence
Bad, need the kieselguhr using acidifying that raw material is extracted, in the present invention, diatomaceous for acidifying
Processing method does not do particularly restriction, such as, sulphuric acid or hydrochloric acid can be used to carry out kieselguhr at acidifying
Reason, under preferable case, described acidifying kieselguhr is to silicon with the hydrochloric acid solution that concentration is 0.1-0.5 weight %
Diatomaceous earth carries out acidification acquisition, and the time of acidification is 10-60min, relative to the silicon of 100g
Diatomaceous earth, the consumption of hydrochloric acid solution is 100-500 milliliter.
The kind of the method provided by the present invention leaching device to completing leach step the most particularly limits
System, such as, leaching process can be carried out in pot for solvent extraction commonly used in the art or extraction cylinder.
In method provided by the present invention, the step of described extraction includes:
(1) Tara seeds pod and/or soybean pod shell are mixed acquisition the first mixture with pure water；
(2) the first mixture is contacted and stir 3-5h with acidifying kieselguhr and obtain the second mixture；
(3) the second mixture is contacted with active hargil and activated carbon and stirs 30-60min and obtains the 3rd
Mixture；
(4) stop stirring and the 3rd mixture is stood 30-60min.
Wherein, in step (1), the method carrying out mixing with pure water by Tara seeds pod and/or soybean pod shell
Have no particular limits, after Tara seeds pod and/or soybean pod shell can be mixed with pure water, add leaching device
In, it is also possible to for Tara seeds pod and/or soybean pod shell are added separately in leaching device with water, and for tower
Soybean pod and/or soybean pod shell is drawn to add the sequencing not requirement of leaching device with water.
In method provided by the present invention, by permissible with the mode that acidifying kieselguhr contacts for the first mixture
For making acidifying kieselguhr and the contact of the first mixture under agitation and sufficiently mixing.
In method provided by the present invention, the side that the second mixture is contacted with active hargil and activated carbon
Formula can be to make active hargil contact with activated carbon and the first mixture and sufficiently mix under agitation
Close, wherein, before contacting with the second mixture, can first active hargil be premixed with activated carbon.
Wherein, in step (4), the purpose stopping stirring and standing the 3rd mixture is for continuing
Continue and Tara seeds pod and/or soybean pod shell are sufficiently extracted and by the way of natural subsidence, makes acidity
Kieselguhr, active hargil and activated carbon fall to bottom leaching device, form filtering layer.
In method provided by the present invention, described extraction is carried out at a temperature of 30-60 DEG C, in order to carry
Tara seeds pod and/or the extracting effect of soybean pod shell in high leaching process, it is preferred that extraction is at 35-55 DEG C
At a temperature of carry out.
In method provided by the present invention, the Tara seeds pod relative to 100g and/or soybean pod shell, described
The consumption of pure water is 1000-3000g, be acidified diatomaceous consumption be 1-5g, the consumption of active hargil be
3-6g, the consumption of activated carbon are 3-6g, preferably in the case of, Tara seeds pod relative to 100g and/or
Soybean pod shell, the consumption of described pure water is 1500-2500g, and being acidified diatomaceous consumption is 1.5-4.5g, work
The consumption of property hargil is 3.5-5.5g, the consumption of activated carbon is 3.5-5.5g.
In the present invention, the diatomaceous granular size of described acidifying is 100-400 mesh, SiO2Content
>=88.5%, the granular size of described active hargil is 100-300 mesh, and activity degree is 120-220, described
Activated carbon is Powdered Activated Carbon, and iodine number is 700-1000mg/g, methylene blue number 120-180mg/g.
In the present invention, in addition to pure water, acid kieselguhr, active hargil and activated carbon used by leaching process
Material can also include that other can adsorb the adsorbent of polysaccharide, protein, gelatin substance, the most poly-
Close aluminum sulfate, aluminium polychlorid, aluminium oxide.
Method provided by the present invention is additionally included in after standing process terminates, and is filtered to remove impurity, it is thus achieved that turbid
The lixiviating solution of degree not higher than 150NTU.Vacuum filtration preferably can be used in order to improve the efficiency of filtration
Mode filters, when use vacuum filtration filter type time, the vacuum of sucking filtration be-0.03MPa～
-0.05MPa。
Method provided by the present invention also includes lixiviating solution carrying out further post-processing step to obtain
Tower draws industrial tannic acid finished product, described post-processing step can include being concentrated in vacuo and being spray-dried, specifically
, described in the method that is concentrated in vacuo for using rotary evaporator, at a temperature of 45-65 DEG C, be concentrated into
Solid content, is being entered to 35-45%, the method for described spray drying for using small-sized spray drier
Air temperature 160-180 DEG C, is spray-dried under conditions of leaving air temp 65-80 DEG C.
After being spray-dried, the outward appearance to the tannic acid product obtained is faint yellow unformed powder, can
To use tannic acid to analyze test method LY/T1642-2005, the parameters of product is analyzed inspection
Survey, analyze the project of detection and include the tannic acid content of sample, loss on drying, water insoluble matter content and
Color.
Hereinafter will be described the present invention by embodiment.In following example:
Pot for solvent extraction is purchased from Shanghai Hui Zhan experimental facilities company limited, model HZ-TQG；
Kieselguhr is purchased from Kowloon, Kunming filtering technique company limited, and the trade mark is clean clear；
Active hargil is purchased from Pingqiao District, District, Xinyang Area, Henan Province city sunlight bentonite factory, and the trade mark is sunlight；
Activated carbon is purchased from the blue sea, Changzhou green technology company limited, and the trade mark is the blue sea；
Following example utilize tannic acid analyze test method LY/T1642-2005 to the list in product
Thujic acid content, loss on drying, water-insoluble and color are analyzed.
Embodiment 1
Weigh 5kg Tara seeds pod shell, Tara seeds pod shell is put into the pot for solvent extraction having added 90kg pure water, opens
Open stirring, be sequentially added into the kieselguhr that 0.15kg is acidified with the hydrochloric acid solution of 0.2% mass concentration in advance,
Stirring and leaching 4h, adds 0.23kg active hargil and 0.23kg activated carbon, is stirred for extracting 45min,
Stop stirring, stand extraction 45min, make kieselguhr, active hargil and activated carbon fully settle, formed
Filtering layer.Stopping extraction, carry out vacuum filtration, vacuum degree control is at-0.04MPa.Obtain after sucking filtration is clear
Clear filtered solution, through being concentrated in vacuo, being spray-dried, obtains tower and draws industrial tannic acid product 2.6kg.
Product appearance is faint yellow unformed powder, detects according to the method for standard LY/T1642-2005,
Tannic acid content 81.35 weight % of product, loss on drying 6.21 weight %, water-insoluble 0.52 weight
%, color 0.6 Luo Weibang unit.
Embodiment 2
Prepare tower according to method same as in Example 1 and draw industrial tannic acid, except for the difference that, used
Tower draws raw material to be Tara seeds pod.
Obtaining tower and draw industrial tannic acid product 2.21kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.86 weight % of product, it is dried and loses
Weigh 6.58 weight %, water-insoluble 0.56 weight %, color 0.6 Luo Weibang unit.
Embodiment 3
Prepare tower according to method same as in Example 1 and draw industrial tannic acid, except for the difference that, used
Tower draws raw material to be Tara seeds pod and Tara seeds pod shell, and the ratio of the two is 1:1.
Obtaining tower and draw industrial tannic acid product 2.3kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.98 weight % of product, it is dried and loses
Weigh 5.67 weight %, water-insoluble 0.53 weight %, color 0.6 Luo Weibang unit.
Embodiment 4
Prepare tower according to method same as in Example 1 and draw industrial tannic acid, except for the difference that, the consumption of water
For 75kg, be acidified diatomaceous consumption be 0.075kg, the consumption of active hargil be 0.175kg, activated carbon
Consumption be 0.175kg.
Obtaining tower and draw industrial tannic acid product 2.59kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 81.33 weight % of product, it is dried and loses
Weigh 5.69 weight %, water-insoluble 0.55 weight %, color 0.6 Luo Weibang unit.
Embodiment 5
Prepare tower according to method same as in Example 1 and draw industrial tannic acid, except for the difference that, the consumption of water
For 125kg, be acidified diatomaceous consumption be 0.225kg, the consumption of active hargil be 0.275kg, activity
The consumption of charcoal is 0.275kg.
Obtaining tower and draw industrial tannic acid product 2.61kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.93 weight % of product, it is dried and loses
Weigh 5.6 weight %, water-insoluble 0.52 weight %, color 0.6 Luo Weibang unit.
Embodiment 6
Prepare tower according to method same as in Example 1 and draw industrial tannic acid, except for the difference that, the consumption of water
For 50kg, be acidified diatomaceous consumption be 0.05kg, the consumption of active hargil be 0.15kg, activated carbon
Consumption is 0.15kg.
Obtaining tower and draw industrial tannic acid product 2.57kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 78.09 weight % of product, it is dried and loses
Weigh 5.77 weight %, water-insoluble 0.69 weight %, color 0.8 Luo Weibang unit.
Embodiment 7
Prepare tower according to method same as in Example 1 and draw industrial tannic acid, except for the difference that, the consumption of water
For 150kg, be acidified diatomaceous consumption be 0.25kg, the consumption of active hargil be 0.3kg, activated carbon
Consumption is 0.3kg.
Obtaining tower and draw industrial tannic acid product 2.64kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 79.86 weight % of product, it is dried and loses
Weigh 6.1 weight %, water-insoluble 0.57 weight %, color 0.7 Luo Weibang unit.
Embodiment 8
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, extract
Carry out at a temperature of 30 DEG C.
Obtaining tower and draw industrial tannic acid product 1.8kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 79.85 weight % of product, it is dried and loses
Weigh 4.39 weight %, water-insoluble 0.56 weight %, color 0.7 Luo Weibang unit.
Embodiment 9
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, extract
Carry out at a temperature of 60 DEG C.
Obtaining tower and draw industrial tannic acid product 2.6kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 78.93 weight % of product, it is dried and loses
Weigh 5.76 weight %, water-insoluble 0.68 weight %, color 0.8 Luo Weibang unit.
Embodiment 10
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, sucking filtration true
Reciprocal of duty cycle is-0.03MPa.
Obtaining tower and draw industrial tannic acid product 2.46kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.02 weight % of product, it is dried and loses
Weigh 6.01 weight %, water-insoluble 0.58 weight %, color 0.7 Luo Weibang unit.
Embodiment 11
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, sucking filtration true
Reciprocal of duty cycle is-0.05MPa.
Obtaining tower and draw industrial tannic acid product 2.62kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 78.86 weight % of product, it is dried and loses
Weigh 5.67 weight %, water-insoluble 0.77 weight %, color 0.7 Luo Weibang unit.
Embodiment 12
Using method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, Jiang Tala is former
Expect that the time that the mixture with pure water contacts with acidifying kieselguhr and stirs is 3h.
Obtaining tower and draw industrial tannic acid product 2.61kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.65 weight % of product, it is dried and loses
Weigh 5.93 weight %, water-insoluble 0.59 weight %, color 0.7 Luo Weibang unit.
Embodiment 13
Using method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, Jiang Tala is former
Expect that the time that the mixture with pure water contacts with acidifying kieselguhr and stirs is 5h.
Obtaining tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.01 weight % of product, it is dried and loses
Weigh 6.02 weight %, water-insoluble 0.57 weight %, color 0.7 Luo Weibang unit.
Embodiment 14
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that add activity white
Mixing time after soil and activated carbon is 30min.
Obtaining tower and draw industrial tannic acid product 2.59kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.33 weight % of product, it is dried and loses
Weigh 6.32 weight %, water-insoluble 0.61 weight %, color 0.8 Luo Weibang unit.
Embodiment 15
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that add activity white
Mixing time after soil and activated carbon is 60min.
Obtaining tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.09 weight % of product, it is dried and loses
Weigh 6.36 weight %, water-insoluble 0.61 weight %, color 0.7 Luo Weibang unit.
Embodiment 16
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, the time except for the difference that stood
For 30min.
Obtaining tower and draw industrial tannic acid product 2.6kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.29 weight % of product, it is dried and loses
Weigh 6.87 weight %, water-insoluble 0.59 weight %, color 0.7 Luo Weibang unit.
Embodiment 17
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, the time except for the difference that stood
For 60min.
Obtaining tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.11 weight % of product, it is dried and loses
Weigh 6.06 weight %, water-insoluble 0.59 weight %, color 0.7 Luo Weibang unit.
Comparative example 1
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, the consumption of water
For 175kg.
Obtaining tower and draw industrial tannic acid product 2.72kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 76.53 weight % of product, it is dried and loses
Weigh 6.65 weight %, water-insoluble 0.57 weight %, color 0.7 Luo Weibang unit.
Comparative example 2
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, be acidified diatom
The consumption of soil is 0.3kg.
Obtaining tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 80.19 weight % of product, it is dried and loses
Weigh 5.96 weight %, water-insoluble 0.9 weight %, color 0.7 Luo Weibang unit.
Comparative example 3
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, active hargil
Consumption be 0.1kg.
Obtaining tower and draw industrial tannic acid product 2.6kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 77.01 weight % of product, it is dried and loses
Weigh 5.31 weight %, water-insoluble 0.67 weight %, color 0.8 Luo Weibang unit.
Comparative example 4
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, activated carbon
Consumption is 0.33kg.
Obtaining tower and draw industrial tannic acid product 2.59kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 76.32 weight % of product, it is dried and loses
Weigh 6.1 weight %, water-insoluble 0.89 weight %, color 0.7 Luo Weibang unit.
Comparative example 5
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, extract
Carry out at a temperature of 65 DEG C.
Obtaining tower and draw industrial tannic acid product 2.64kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 77.69 weight % of product, it is dried and loses
Weigh 8.39 weight %, water-insoluble 0.88 weight %, color 0.8 Luo Weibang unit.
Comparative example 6
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, sucking filtration true
Reciprocal of duty cycle is-0.06MPa
Obtaining tower and draw industrial tannic acid product 2.68kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 77.98 weight % of product, it is dried and loses
Weigh 5.4 weight %, water-insoluble 0.81 weight %, color 0.7 Luo Weibang unit.
Comparative example 7
Using method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that, Jiang Tala is former
Expect that the time that the mixture with pure water contacts with acidifying kieselguhr and stirs is 2.5h.
Obtaining tower and draw industrial tannic acid product 2.4kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 76.88 weight % of product, it is dried and loses
Weigh 8.6 weight %, water-insoluble 0.8 weight %, color 0.7 Luo Weibang unit.
Comparative example 8
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, except for the difference that add activity white
Mixing time after soil and activated carbon is 25min.
Obtaining tower and draw industrial tannic acid product 2.56kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 76.49 weight % of product, it is dried and loses
Weigh 8.4 weight %, water-insoluble 0.64 weight %, color 0.7 Luo Weibang unit.
Comparative example 9
Use method same as in Example 1 to prepare tower and draw industrial tannic acid, the time except for the difference that stood
For 25min.
Obtaining tower and draw industrial tannic acid product 2.58kg, product appearance is faint yellow unformed powder, according to
The method detection of standard LY/T1642-2005, tannic acid content 76.56 weight % of product, it is dried and loses
Weigh 7.65 weight %, water-insoluble 0.76 weight %, color 0.7 Luo Weibang unit.
By the result of embodiment 1-17 it can be seen that utilize production method provided by the present invention to prepare tower
Draw industrial tannic acid can obtain meeting the product of LY/T1642-2005 standard.And the tannic acid of product
Content is higher than 78.0 weight %, and loss on drying is less than 9.0 weight %, and water-insoluble is less than 0.8 weight %,
Color is less than 3.0 Luo Weibang units.
By the result of embodiment 1,4 and 5 and embodiment 6 and 7 it can be seen that when water consumption,
Be acidified diatomaceous consumption, the consumption of active hargil, activated carbon consumption the present invention preferred scope it
Time interior, it is thus achieved that the tannic acid content of product higher, water insoluble matter content is lower, and color is more shallow.
By the result of embodiment 1 and comparative example 1 it can be seen that when amount of water is 175kg, i.e. soak
When amount of water is too much, it is thus achieved that the tannic acid content step-down of product, illustrate to add water a certain amount of after, tannin
Acid Leaching-out Ratio does not continue with the increase of the water yield to raise, and is now further added by the water yield, only results in more
Impurity leaches.
By the result of embodiment 1 and comparative example 2 it can be seen that when acidifying kieselguhr consumption increases to
During 0.3kg, it is thus achieved that tannic acid content, water-insoluble and the color of product the most undesirable, instruction sheet
Thujic acid can be acidified the impurity of diatomite adsorption be have a certain amount of, when acidifying kieselguhr is these impurity
Completely after absorption, it is further added by diatomaceous amount, has not had positive meaning, be kieselguhr basis on the contrary
The impurity effect that body the is carried quality of product.
By the result of embodiment 1 and comparative example 3 it can be seen that when active hargil consumption is 0.1kg,
The tannic acid content of the product obtained is 77.01%, does not reaches the requirement of more than 78.0%, illustrates that activity is white
The addition deficiency of soil can cause the reduction of tannic acid content.
By the result of embodiment 1 and comparative example 4 it can be seen that working as activated carbon dosage is 0.33kg, and
When excess adds activated carbon, it is thus achieved that the quality of product not as by optimum usage amount interpolation activated carbon gained
Product, the impurity being tightly held by activated carbon in instruction sheet thujic acid be have a certain amount of, when activated carbon is these
After impurity adsorbs completely, it is further added by the amount of activated carbon, has not had positive meaning, be activity on the contrary
The impurity effect that charcoal itself the is carried quality of product.
By the result of embodiment 1 and comparative example 5 it can be seen that when extraction temperature is 65 DEG C, it is thus achieved that
Tannic acid content, water-insoluble and the color of product be all worse than the product of gained in the range of normal extraction temperature
Product, illustrate that the too high quality to tannic acid of extraction temperature causes harmful effect.
By the result of embodiment 1 and comparative example 6 it can be seen that working as sucking filtration vacuum is-0.06MPa
Time, it is thus achieved that the quality of product not as the product by optimum vacuum sucking filtration, when sucking filtration is described, vacuum is spent
Height, can cause a certain amount of impurity to wear filter, affect the quality of tannic acid.
By the result of embodiment 1 and comparative example 7 it can be seen that work as the mixing that tower is drawn raw material and pure water
Thing with acidifying kieselguhr time of contacting and stirring in the scope given by the present invention time, it is thus achieved that tannin
The quality of acid is higher.
By the result of embodiment 1 and comparative example 8 it can be seen that when after interpolation active hargil and activated carbon
Mixing time in the scope given by the present invention time, it is thus achieved that the quality of tannic acid higher.
It is in institute of the present invention it can be seen that work as the time stood by the result of embodiment 1 with comparative example 9
Time in the range of being given, it is thus achieved that the quality of tannic acid higher.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited to above-mentioned reality
Execute the detail in mode, in the technology concept of the present invention, can be to the technical side of the present invention
Case carries out multiple simple variant, and these simple variant belong to protection scope of the present invention.Additionally need
Each concrete technical characteristic bright, described in above-mentioned detailed description of the invention, in reconcilable feelings
Under condition, can be combined by any suitable means in order to avoid unnecessary repetition, the present invention couple
Various possible compound modes illustrate the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as its
Without prejudice to the 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 characterised in that the method includes with acidifying
Kieselguhr, active hargil and activated carbon obtain lixiviating solution after extracting Tara seeds pod and/or soybean pod shell；
Wherein, the step of described extraction includes:
(1) Tara seeds pod and/or soybean pod shell are mixed acquisition the first mixture with pure water；
(2) the first mixture is contacted and stir 3-5h with acidifying kieselguhr and obtain the second mixture；
(3) the second mixture is contacted with active hargil and activated carbon and stirs 30-60min and obtains the 3rd
Mixture；
(4) stop stirring and the 3rd mixture is stood 30-60min.
Tower the most according to claim 1 draws the preparation method of industrial tannic acid, wherein, relative to
The Tara seeds pod of 100g and/or soybean pod shell, the consumption of described pure water is 1000-3000g, is acidified kieselguhr
Consumption be 1-5g, the consumption of active hargil be 3-6g, the consumption of activated carbon be 3-6g.
Tower the most according to claim 2 draws the preparation method of industrial tannic acid, wherein, relative to
The Tara seeds pod of 100g and/or soybean pod shell, the consumption of described pure water is 1500-2500g, is acidified kieselguhr
Consumption be 1.5-4.5g, the consumption of active hargil be 3.5-5.5g, the consumption of activated carbon be 3.5-5.5g.
Tower the most according to claim 1 draws the preparation method of industrial tannic acid, wherein, described tower
Drawing the fruit that soybean pod draws tree to be tied by tower, including soybean pod shell and seed, described Tara seeds pod shell is Tara seeds
Pod removes the part after seed.
5. according to the method that tower draws industrial tannic acid of preparing described in claim 1 or 4, wherein, institute
State Tara seeds pod to be the complete Tara seeds pod without pulverization process or be more than for particle diameter after pulverizing
The Tara seeds pod of 1 × 1cm；
Wherein, described Tara seeds pod shell is the complete Tara seeds pod shell without pulverization process or is to pass through
The particle diameter Tara seeds pod shell more than 1 × 1cm after pulverizing.
6. the preparation side of industrial tannic acid is drawn according to the tower described in any one in claim 1,2 and 4
Method, wherein, described acidifying kieselguhr is to enter kieselguhr with the hydrochloric acid solution that concentration is 0.1-0.5 weight %
Row acidification obtains, and the time of acidification is 10-60min, relative to the kieselguhr of 100g,
The consumption of hydrochloric acid solution is 100-500 milliliter.
7. the preparation method of industrial tannic acid is drawn according to the tower described in claim 1,2 or 4, wherein,
Described extraction is carried out at a temperature of 30-60 DEG C.
Tower the most according to claim 5 draws the preparation method of industrial tannic acid, wherein, described leaching
Carry and carrying out at a temperature of 30-60 DEG C.
Tower the most according to claim 1 draws the preparation method of industrial tannic acid, wherein, the method
It is additionally included in and the 3rd mixture is stood 30-60min final vacuum sucking filtration acquisition lixiviating solution, the vacuum of sucking filtration
Degree is-0.03MPa～-0.05MPa.
Tower the most according to claim 1 draws the preparation method of industrial tannic acid, wherein, the method
Also include that the filtered solution obtaining vacuum filtration concentrates and is dried.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2088590A (en) * | 1936-07-30 | 1937-08-03 | Merck & Co Inc | Stabilized aqueous solution of tannic acid |
| CN101838294A (en) * | 2010-04-07 | 2010-09-22 | 云南瑞宝生物科技有限公司 | Method for preparing high-purity Tara tannic acid |
| CN102140121A (en) * | 2010-01-28 | 2011-08-03 | 中国林业科学研究院林产化学工业研究所 | Preparation method of tara industrial tannic acid |
| CN102786554A (en) * | 2012-08-10 | 2012-11-21 | 刀海林 | Method for preparation of industrial tannic acid with Tara as raw material in supercritical carbon dioxide |
| CN103122011A (en) * | 2013-03-20 | 2013-05-29 | 广西壮族自治区林业科学研究院 | Method for preparing high-purity tannic acid by utilizing tara |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5163199A (en) * | 1974-11-22 | 1976-06-01 | Fuji Chem Ind Co Ltd | TANNINSANNOSEIZOHOHO |
-
2013
- 2013-09-04 CN CN201310397932.XA patent/CN103408608B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2088590A (en) * | 1936-07-30 | 1937-08-03 | Merck & Co Inc | Stabilized aqueous solution of tannic acid |
| CN102140121A (en) * | 2010-01-28 | 2011-08-03 | 中国林业科学研究院林产化学工业研究所 | Preparation method of tara industrial tannic acid |
| CN101838294A (en) * | 2010-04-07 | 2010-09-22 | 云南瑞宝生物科技有限公司 | Method for preparing high-purity Tara tannic acid |
| CN102786554A (en) * | 2012-08-10 | 2012-11-21 | 刀海林 | Method for preparation of industrial tannic acid with Tara as raw material in supercritical carbon dioxide |
| CN103122011A (en) * | 2013-03-20 | 2013-05-29 | 广西壮族自治区林业科学研究院 | Method for preparing high-purity tannic acid by utilizing tara |
Non-Patent Citations (4)
| Title |
|---|
| 单宁的提取纯化技术研究进展;王红等;《辽宁化工》;20110831;第40卷(第8期);第864-870页 * |
| 塔拉单宁提取和精制工艺对络合沉锗率影响;秦清等;《林产化学与工业》;20120430;第32卷(第2期);第79-82页 * |
| 物理吸附法提纯五倍子单宁的研究;徐浩等;《林产化学与工业》;20081231;第28卷(第6期);第79-82页 * |
| 膜分离与改性活性炭吸附组合技术制备高纯单宁酸的研究;张太龙;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20070615;B016-69页 * |
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