CN108929391A - A kind of purification process of synanthrin extracting solution - Google Patents
A kind of purification process of synanthrin extracting solution Download PDFInfo
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- CN108929391A CN108929391A CN201810816434.7A CN201810816434A CN108929391A CN 108929391 A CN108929391 A CN 108929391A CN 201810816434 A CN201810816434 A CN 201810816434A CN 108929391 A CN108929391 A CN 108929391A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0051—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Fructofuranans, e.g. beta-2,6-D-fructofuranan, i.e. levan; Derivatives thereof
- C08B37/0054—Inulin, i.e. beta-2,1-D-fructofuranan; Derivatives thereof
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Abstract
The present invention relates to a kind of purification process of synanthrin extracting solution, which includes alkalization, phosphoric acid processing, is separated by solid-liquid separation.Purification process of the invention reduces 60% or more base amount than the prior art, flocculate precipitate after can making synanthrin solution purification simultaneously is formed with raw material/ingredient beneficial to feed or organic fertilizer production, to thoroughly solve problem of environmental pollution caused by the solid waste product that previous purified inulin solution is formed.
Description
[technical field]
The invention belongs to food ingredient or medical material production technical fields, more particularly it relates to a kind of synanthrin
The purification process of extracting solution or synanthrin solution.
[background technique]
Synanthrin also known as levulan or inulin are by fructosyl through β-glucosides key connection, the levulan that the degree of polymerization is 2~60,
Its molecular formula C6H11O5(C6H10O5)nOH, synanthrin are a kind of water-soluble dietary fibers, and can be used as food or raw-food material makes
With the raw material that also can be used as the industries such as medicine, feed or cosmetics use.
Nature has up to more than 3,000 kind plants all to contain levulan (synanthrin), wherein with jerusalem artichoke (alias Jerusalem artichoke) or witloof
Content be height, be all industrially using both crop tubers as raw material therefore, cleaned, broken, hot water extracts, purification etc.
Synanthrin syrup or inulin product is made in process.
In general, jerusalem artichoke or endive or stem tuber extract synanthrin ingredient therein with hot water after crushing, to obtain chrysanthemum
Sugared extracting solution, solid content is usually 5%~25% in extracting solution, and in synanthrin extracting solution also containing soluble protein,
The ingredients such as pectin, organic acid, pigment, these ingredients generally are regarded as impurity component, in extracting solution its total content be about 0.5~
2.5%.Therefore it must be removed to obtain the scavenging solution of synanthrin.
At present in industrialized production, removes these impurity and generally use lime-carbonatation process and/or Acetic, i.e., in synanthrin
Calcium oxide or calcium hydroxide are added in extracting solution, the pH value of extracting solution is adjusted to strong basicity, to reach protein, pectin class object
The isoelectric point of matter, to make protein, pectic substance is flocculated；Then be added carbonic acid or carbon dioxide and/or acetic acid into
Row neutralizes, the precipitatings such as calcium carbonate that neutralization reaction generates not only can adsorpting pigment substance, protein and pectin can also be flocculated
Object is reunited, and filter operation sediment separate out and flocculate is then utilized, to be purified the synanthrin solution of (purification).
CN 104844733A discloses the production technology that the pure natural inulin of high-purity is extracted from jerusalem artichoke, purification therein
Decolorization process is: synanthrin liquid being heated to 75 degree, adds milk of lime, is stirred, adjusts pH value to 11-12, the time 30 minutes, allows protein
It separates out；The ice acetic acid in purification pot adjusts pH value to 7, the time 15 minutes；Continue to add active carbon decoloring in purification pot, protect
75 degree of temperature are held, the time 30 minutes, is sufficiently stirred, plate and frame filter press is finally pumped by liquid glucose and albumen, Activated carbon separation, will divide
Synanthrin liquid pump from after enters temporary storage tank；Since protein belongs to impurity component in synanthrin, so to add lime except deproteinized；It is on the rocks
Acetic acid is in order to which material is pulled back to neutrality；Active carbon is added to seek to remove most of pigment in liquid glucose.
In existing lime-carbonatation process/or Acetic purification process, to improve the effect of purifying and being to realize solution
Liquid-solid be separated by filtration, it is necessary to be added excessive alkali (lime), the additional amount of alkali will usually reach synanthrin and extract liquid measure
1.5% or more, even up to 2% or more, the consumption of alkali is big；Simultaneously the flocculate that is separated by filtration out be calcium carbonate and/or
Calcium acetate and its protein of absorption, the organic matters such as pectin class and pigment, this mixture are the products that can not be utilized, usually
Handled with land-fill method, caused by problem of environmental pollution it is more serious.
Therefore, the present inventor is directed to prior art situation, is summarizing on prior art basis, is passing through lot of experiments
With commerical test, the present invention is completed finally.
[summary of the invention]
[technical problems to be solved]
The object of the present invention is to provide a kind of purification process of synanthrin extracting solution.
[technical solution]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of purification process of synanthrin extracting solution.
The step of synanthrin extracting solution purification process, is as follows:
A, it alkalizes
Alkaline earth oxide or alkaline earth metal hydroxide are added into synanthrin extracting solution, make the synanthrin extracting solution
PH value reaches 10 or more, and 10~40min of quaternization is then carried out under conditions of 30~65 DEG C of temperature, obtains a kind of alkalization chrysanthemum
Sugared extracting solution；
B, phosphoric acid is handled
Under conditions of 65~100 DEG C of temperature, adding phosphoric acid into the alkalization synanthrin extracting solution that step A is obtained makes chrysanthemum of alkalizing
The pH value of sugared extracting solution reaches 6~8, then carries out 15~40min of neutralization reaction, obtains a kind of neutralization synanthrin extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while the past neutralization synanthrin extracting solution
Whether middle addition flocculant or not, and 20~90min of sedimentation separation obtains a kind of purified inulin solution.
A preferred embodiment of the invention, in step, the alkaline earth oxide be calcium oxide or
Magnesia；The alkaline earth metal hydroxide is calcium hydroxide or magnesium hydroxide.
According to another preferred method of implementation of the present invention, in step, the pH value of the synanthrin extracting solution reaches 10.0
~12.0.
According to another preferred method of implementation of the present invention, in stepb, the concentration of the phosphoric acid is 5~75%.
According to another preferred method of implementation of the present invention, in stepb, inorganic acid can be added while adding phosphoric acid
Or organic acid；The inorganic acid is sulfuric acid, sulfurous acid or boric acid；The organic acid is acetic acid, propionic acid, citric acid or grass
Acid.
According to another preferred method of implementation of the present invention, in stepb, the molar ratio of phosphoric acid and inorganic acid or organic acid
It is 1:1~9.
According to another preferred method of implementation of the present invention, in step C, the flocculant is one or more is selected from
Aluminium polychloride, aluminum chloride hydrocarbon complex, zinc polysilicate, bodied ferric sulfate, polyacrylamide or chitosan flocculant.According to
Different flocculant requirements is both needed to be configured to weak solution to be subject to using the additive amount of usual flocculant is to neutralize synanthrin and mention
Liquid weight is taken to be calculated as 0.001~0.01%.
According to another preferred method of implementation of the present invention, in step C, the precipitating flocculate that sedimentation separation obtains is direct
For the ingredient of feed or the raw material of organic fertilizer.
According to another preferred method of implementation of the present invention, in step C, the precipitating flocculate that sedimentation separation obtains passes through
For the ingredient of feed or the raw material of organic fertilizer after filter and/or drying.
The present invention is described in more detail below.
The present invention relates to a kind of synanthrin extracting solution purification process.
The step of synanthrin extracting solution purification process, is as follows:
A, it alkalizes
Alkaline earth oxide or alkaline earth metal hydroxide are added into synanthrin extracting solution, make the synanthrin extracting solution
PH value reaches 10 or more, and 10~40min of quaternization is then carried out under conditions of 30~65 DEG C of temperature, obtains a kind of alkalization chrysanthemum
Sugared extracting solution；
The synanthrin extracting solution that the present invention uses is that witloof chopping is added hot water to make its dissolution, also can will be after jerusalem artichoke defibrination
Water hot extraction is added, obtains a kind of brownish black liquid, the common solid content of the extracting solution is by weight 10.0~15%,
Wherein impurity content 1.0~2.2%.
Alkaline earth oxide is added into synanthrin extracting solution or the purpose of alkaline earth metal hydroxide is, synanthrin is mentioned
The pH value of liquid is taken to be adjusted to 10.0 or more, it is preferable that the pH value of the synanthrin extracting solution reaches 10.0~12.0, reaches wherein egg
White matter, the isoelectric point of pectic substance simultaneously are allowed to agglomerate, and then neutralizing solution makes wherein alkaline-earth metal ions Precipitation, they
Meeting adsorpting pigment substance, while the flocculate of protein and pectin further being made to reunite.
According to the present invention, the alkaline earth oxide is calcium oxide or magnesia；The alkaline-earth metal hydroxide
Object is calcium hydroxide or magnesium hydroxide, they are all current market sales of products.Certainly, the present invention also can be used other
Basic anhydride or alkaline hydrated oxide, only these basic anhydride or alkaline hydrated oxide can be by the pH of synanthrin extracting solution
Value, which is adjusted, does not have any detrimental effect to 10.0 or more, and to alkalinization step and its subsequent step, these basic anhydride
Or alkaline hydrated oxide is also all within protection scope of the present invention.
In the present invention, quaternization temperature is preferably 35~45 DEG C.In fact, the quaternization temperature it is higher or
It is some more low be all it is desirable, except to extract it is basified when solution color value have an impact in addition to, it is any unfavorable not generate to subsequent step
Influence.
In the present invention, the quaternization time is preferably 15~30min.In fact, the quaternization time can be more
It is long, can also be shorter, in addition to the volume to production equipment has an impact, alkalinization step and its subsequent step will not be generated and appointed
What detrimental effect.
In the present invention, alkaline earth oxide or alkaline earth metal hydroxide addition manner do not specially require, can be with
Disposable addition, can also substep or repeatedly addition.
Equipment used in this alkalinization step is all usually used in the art or configuration temperature is controlled, stirred
The hybrid reactor of the affiliated facilities such as device, feeding device is mixed, these reactors are also current market sales of product, example
The 5000L Tai Ji board enamel reaction still such as produced by Shandong Zibo Tai Ji industrial enamel Co., Ltd.
In the present invention, the pH value of the synanthrin extracting solution is measured using analysis PH instrument, also uses special pH test paper
Carry out auxiliary measuring.
B, phosphoric acid is handled
Under conditions of 65~100 DEG C of temperature, adding phosphoric acid into the alkalization synanthrin extracting solution that step A is obtained makes chrysanthemum of alkalizing
The pH value of sugared extracting solution reaches 6~8, then carries out 15~40min of neutralization reaction, obtains a kind of neutralization synanthrin extracting solution；
Synanthrin extracting solution purification process of the present invention is to replace previous carbonic acid/or acetic acid to be neutralized with phosphoric acid, to have
Effect ground solves the problems, such as existing for previous carbonatation process/or Acetic two.Firstly, to reach solution final for lime usage amount of the invention
Isoelectric point (pH value 10.5~11.5) is added without excessive, and such lime consumption is generally only the pact that synanthrin extracts liquid measure
0.2%~0.5%, 60% or more base amount is reduced than existing method；Secondly, calcium phosphate precipitation and its organic-flocculation object are good
Feed or organic fertilizer production raw material, then thoroughly solve problem of environmental pollution caused by calcium carbonate-organic matter solid waste.
The present invention is by weight 5~75%, preferably 10~50% using the concentration of phosphoric acid.Certainly, phosphoric acid concentration
Can be higher, can also be some more low, only these phosphoric acid concentrations can guarantee that the pH value for making to alkalize synanthrin extracting solution reaches 6~8,
6.0~7.0 are preferably reached, and does not have any detrimental effect to subsequent step and its product.
In the present invention, added while adding phosphoric acid inorganic acid or organic acid purpose be during auxiliary phosphoric acid carries out and
Precipitation reaction, to change the type of alkali salt in sediment, improve the sinking speed of sediment and the filterability of sediment
It can, further increase impurity removal percentage and expand the purposes of sediment.
In the present invention, the inorganic acid is sulfuric acid, sulfurous acid (sulfur dioxide) or boric acid；The organic acid is second
Acid, propionic acid, citric acid or oxalic acid.
In the present invention, the molar ratio of phosphoric acid and inorganic acid or organic acid is 1:1~9, excessively very few all to lose this hair
Benefit brought by bright phosphoric acid method itself.
In the present invention, neutralization reaction temperature is preferably 80~95 DEG C.In fact, the temperature of neutralization reaction it is higher or
It is some more low be all it is feasible, temperature it is too low only will affect precipitating flocculate sinking speed, it is excessively high, increase equipment investment at
This, but not negative effect is generated to the benefit of this method.
In the present invention, which is preferably 20~30min.In fact, the neutralization reaction time can be with
It is longer, can also be shorter, but the too long neutralization reaction time, such as the neutralization reaction time was at 2 hours or more, it will cause
Flocculated protide, the redissolution of pectin constituents return in synanthrin solution, reduce so as to cause the removal efficiency of impurity, are undesirable
's.
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while the past neutralization synanthrin extracting solution
Whether middle addition flocculant or not, and 20~90min of sedimentation separation obtains a kind of purified inulin solution.
In the present invention, the synanthrin extracting solution of neutralization carries out liquid-solid phase separation using flocculating setting mode, obtains limpid
Synanthrin solution and sticky flocculate precipitate are purified, just efficiently solves what calcium phosphate flocky precipitate was difficult to directly to filter in this way
Professional problem can continue to be processed into the ingredient of feed or the original of fertilizer containing calcium phosphate and organic matter flocculate precipitate simultaneously
Material.
According to the present invention, the main purpose that flocculant is added into the neutralization synanthrin extracting solution is to improve calcium phosphate wadding
The sinking speed of shape sediment, including the sedimentation separation speed of organic flocculate and calcium of organic acid, flocculant need to be configured to
PPM grades of weak solutions are subject to using the additive amount of flocculant is to be calculated as 0.001~0.01% with the weight of synanthrin solution extracting solution.
The flocculant that the present invention uses be it is one or more selected from aluminium polychloride, aluminum chloride hydrocarbon complex, zinc polysilicate,
The flocculant of bodied ferric sulfate, polyacrylamide or chitosan.These flocculants are all current market sales of products, such as
The PAC01 aluminium polychloride produced by Wuxi Lan Bo Chemical Company, PFS bodied ferric sulfate, APAM anionic poly- third
Acrylamide, by Nantong it is emerging at biological Co., Ltd production the dedicated chitosan flocculant of protein, Hubei flourishing age environmental protection company pin
The poly aluminium iron silicate etc. sold.
In the present invention, if the shorter synanthrin solution sedimentation separation time in settlement separator the better, if sedimentation point
It is longer than 2 hours from the time, then the organic matter for flocculating out will more be redissolved in solution, and purification efficiency is caused to reduce, and be practiced
It proves, it is reasonable that synanthrin solution sedimentation separation time in settlement separator, which is 20~90min,.
The settlement separator that the present invention uses is various sedimentation separation equipment usually used in the art, for this
For invention, the sedimentation separation time, The faster the better, and to avoid more organic-flocculation object back dissolvings in solution, such as the present invention can
To use clearance-type or continous way settlement separator, wherein be preferred with vertical conical gravity two-phase settlement separator, can efficiently by
Precipitating flocculate is separated with synanthrin scavenging solution, the synanthrin solution being purified.
According to the present invention, the thick shape precipitating flocculate that sedimentation separation obtains contains calcium phosphate and organic matter flocculate, it can
To be directly used in the ingredient of feed or the raw material of organic fertilizer, or for the ingredient or organic of feed after filtration and or drying
The raw material of fertilizer.
In the prior art, the flocculate precipitate of synanthrin extracting solution generallys use filter type and is separated, and generally uses
Plate and frame filter is filtered, and not only quantity is big for obtained calcium carbonate-organic matter sediment, and only calcium oxide additional amount is usual
1.5%~2.0% be up in terms of synanthrin solution weight, and one of the problem of can not be used, become environmental pollution.
Synanthrin extracting solution purification process of the present invention has the characteristics that following:
1. the dosage of synanthrin extracting solution purification process alkali (calcium oxide or calcium hydroxide) of the present invention reaches solution finally equal electricity
Point is added without excessive, and such base amount is 0.2%~0.5% that synanthrin extracts liquid measure, reduces alkaline consumption dosage 60%
More than.
2. the method for the present invention replaces the alkaline matter in carbonic acid/or acetic acid and being added with phosphoric acid, calcium phosphate obtained is heavy
It forms sediment and its organic-flocculation object is good feed or organic fertilizer raw material, it is dirty thoroughly to solve calcium carbonate-organic matter solid waste environment
Dye problem.
3. due to the solubility product (10 of calcium phosphate precipitation-29Power grade) it is far smaller than the solubility product (10 of calcium carbonate-9Power
Grade), alkaline-earth metal ions can be made to precipitate using phosphoric acid more complete, the alkaline-earth metal ions content for purifying synanthrin solution is usually small
Effectively avoid synanthrin industrial far below the remaining alkaline-earth metal ions amount of 250~400mg/L of existing carbonatation process in 100mg/L
Equipment scaling problem during metaplasia produces.
[beneficial effect]
The beneficial effects of the present invention are: reducing alkaline consumption dosage 60% than existing method in the comparable situation of clean-up effect
More than；Turn waste into wealth simultaneously, so that flocculate precipitate is become the raw material of good feed or organic fertilizer production, thoroughly solve carbonic acid
Calcium-organic matter solid waste problem of environmental pollution；In addition equipment scaling problem in industrial processes can also effectively be avoided.
[specific embodiment]
It will be better understood that the present invention by following embodiments, use batch process or continuity method in actual production process
Operation operation, is no difference substantial effect of the invention.
Embodiment 1: synanthrin extracting solution purifying
The implementation steps of the embodiment are as follows:
A, it alkalizes
It is by weight 12.0%, adds in the synanthrin extracting solution of impurity content 1.4% toward pH value 6.7, solid object content
Adding ratio of water to material is the calcium oxide emulsion of 5:1, so that the pH value of synanthrin extracting solution is reached 10.5, wherein calcium oxide additional amount is
The 0.32% of synanthrin amount of solution carries out quaternization 25min under conditions of 42 DEG C of temperature, obtains a kind of alkalization synanthrin extraction
Liquid；
B, phosphoric acid is handled
Under conditions of 80 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
40% phosphoric acid makes the pH value of alkalization synanthrin extracting solution reach 6.6, then carries out neutralization reaction 15min, obtains a kind of neutralization synanthrin
Extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, sedimentation separation 50min, separator top
Lurid purification synanthrin solution is obtained, uses the measurement of K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer to be
86.5%, the precipitating flocculate that lower part sedimentation separation obtains directly is mixed and made into the original of the feed rich in protein with corn stalk powder
Material.
Embodiment 2: synanthrin extracting solution purifying
The implementation steps of the embodiment are as follows:
A, it alkalizes
It is by weight 11.0%, adds in the synanthrin extracting solution of impurity content 1.2% toward pH value 6.5, solid object content
The calcium oxide emulsion for adding embodiment 1 to use, gradually makes the pH value of synanthrin extracting solution reach 11.5, and wherein calcium oxide additional amount is
The 0.41% of synanthrin amount of solution carries out quaternization 30min under conditions of 30 DEG C of temperature, obtains a kind of alkalization synanthrin extraction
Liquid；
B, phosphoric acid is handled
Under conditions of 95 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
30% phosphoric acid makes the pH value of alkalization synanthrin extracting solution reach 6.5, then carries out neutralization reaction 30min, obtains a kind of neutralization synanthrin
Extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, sedimentation separation 65min, separator top
Lurid purification synanthrin liquid is obtained, uses the measurement of K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer for 88%,
The precipitating flocculate that lower part sedimentation separation obtains directly is mixed and made into the feedstuff rich in protein with corn stalk powder.
Embodiment 3: synanthrin extracting solution purifying
The implementation steps of the embodiment are as follows:
A, it alkalizes
It is by weight 11.50%, adds in the synanthrin extracting solution of impurity content 1.7% toward pH value 6.6, solid object content
The calcium oxide emulsion for adding embodiment 1 to use, gradually makes the pH value of synanthrin extracting solution reach 11.5, and wherein calcium oxide additional amount is
The 0.37% of synanthrin amount of solution carries out quaternization 40min under conditions of 35 DEG C of temperature, obtains a kind of alkalization synanthrin extraction
Liquid；
B, phosphoric acid is handled
Under conditions of 90 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
20% phosphoric acid makes the pH value of alkalization synanthrin extracting solution reach 7.4, then carries out neutralization reaction 25min, obtains a kind of neutralization synanthrin
Extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while being added by neutralize synanthrin extraction
The flocculant of 5% bodied ferric sulfate of liquid poidometer and 0.5% chitosan mixture, flocculant solution additive amount are to neutralize synanthrin to extract
The 1.5% of liquid weight is uniformly mixed, and then sedimentation separation 90min, obtains the purification synanthrin solution of light yellow clear, is used
For the measurement of K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer for 88.5%, precipitating flocculate obtained after separation is straight
It connects and is mixed with bagasse powder rich in calcium phosphate-protein feedstuff.
Embodiment 4: synanthrin extracting solution purifying
The implementation steps of the embodiment are as follows:
A, it alkalizes
It is by weight 11.0%, adds in the synanthrin extracting solution of impurity content 1.3% toward pH value 6.6, solid object content
The calcium oxide emulsion for adding embodiment 1 to use, makes the pH value of synanthrin extracting solution reach 11.5, and wherein calcium oxide additional amount is synanthrin
The 0.3% of amount of solution then carries out quaternization 30min under conditions of 38 DEG C of temperature, obtains a kind of alkalization synanthrin extracting solution；
B, phosphoric acid is handled
Under conditions of 100 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
20% phosphoric acid makes the pH value of alkalization synanthrin extracting solution reach 6.0, then carries out neutralization reaction 35min, obtains a kind of neutralization synanthrin
Extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while being added to neutralize synanthrin extracting solution
5% aluminium chloride of poidometer and 0.1% anion-polyacrylamide flocculant, flocculant solution additive amount are to neutralize synanthrin
The 0.7% of extracting solution weight is uniformly mixed, and then sedimentation separation 80min, obtains the purification synanthrin solution of light yellow clear, adopt
It is measured with K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer as 90.5%；Precipitating flocculate obtained after separation
It mixes with wheat stalk powder, and is made after rotary vacuum filter suction strainer rich in calcium phosphate-organic matter fertilizer.
Embodiment 5: synanthrin extracting solution purifying
The implementation steps of the embodiment are as follows:
A, it alkalizes
It is by weight 14.5%, adds in the synanthrin extracting solution of impurity content 1.9% toward pH value 6.5, solid object content
Adding ratio of water to material is the calcium oxide emulsion of 5:2, and the pH value of synanthrin extracting solution is made to reach 11.0, and wherein calcium oxide additional amount is synanthrin
The 0.42% of amount of solution carries out quaternization 25min under conditions of temperature 50 C, obtains a kind of alkalization synanthrin extracting solution；
B, phosphoric acid is handled
Under conditions of 90 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
20% phosphoric acid, while by phosphorus: sulphur molar ratio 1:4 is passed through sulfur dioxide gas (sulfurous acid), reaches the pH value of synanthrin extracting solution
To 7.0, then neutralization reaction 35min is carried out, obtains a kind of neutralization synanthrin extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while being added to neutralize synanthrin extracting solution
The anion-polyacrylamide flocculant of poidometer 0.1%, then sedimentation separation 20min, it is net to obtain extremely lurid synanthrin
Change liquid, uses the measurement of K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer for 91%；Precipitating wadding obtained after separation
Condensate is directly made rich in calcium phosphate-calcium sulfite-organic matter organic fertilizer after rotary vacuum filter suction strainer；The filtrate of suction strainer is clear
It is clear, it can directly recycle.
Embodiment 6: synanthrin extracting solution purifying
A, it alkalizes
It is by weight 9.5%, added in the synanthrin extracting solution of impurity content 0.9% toward pH value 6.8, solid object content
Ratio of water to material is the milk of magnesia of 5:1, and the pH value of synanthrin extracting solution is made to reach 11.0, and wherein magnesia additional amount is synanthrin solution
The 0.28% of amount carries out quaternization 10min under conditions of 65 DEG C of temperature, obtains a kind of alkalization synanthrin extracting solution；
B, phosphoric acid is handled
Under conditions of 65 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
20% phosphoric acid, while pressing phosphorus: the boric acid solution that concentration is by weight 5% is added in boron molar ratio 1:2, makes synanthrin extracting solution
PH value reaches 6.5, then carries out neutralization reaction 30min, obtains a kind of neutralization synanthrin extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while being added to neutralize synanthrin extracting solution
0.1% anion-polyacrylamide flocculant of poidometer, then sedimentation separation 30min to get arrive light yellow and transparent chrysanthemum
Sugared scavenging solution uses the measurement of K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer for 89%；It is obtained after separation heavy
Shallow lake flocculate can be made into the organic fertilizer rich in boron P elements and organic matter after wheat stalk powder is added.
Embodiment 7: synanthrin extracting solution purifying
A, it alkalizes
It is by weight 10.5%, adds in the synanthrin extracting solution of impurity content 1.4% toward pH value 6.7, solid object content
Adding ratio of water to material is the calcium hydroxide emulsion of 5:1, and the pH value of synanthrin extracting solution is made to reach 11.0, and wherein calcium hydroxide additional amount is chrysanthemum
The 0.3% of sugar juice amount carries out quaternization 30min under conditions of temperature 45 C, obtains a kind of alkalization synanthrin extracting solution；
B, phosphoric acid is handled
Under conditions of 75 DEG C of temperature, it is by weight that concentration is added into the alkalization synanthrin extracting solution that step A is obtained
20% phosphoric acid, while pressing phosphoric acid: the citric acid solution that concentration is by weight 20% is added in citric acid molar ratio 1:2, makes chrysanthemum
The pH value of sugared extracting solution reaches 8.0, then carries out neutralization reaction 40min, obtains a kind of neutralization synanthrin extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in settlement separator, while being added by neutralize synanthrin extraction
The flocculant of 5% aluminium chloride of liquid poidometer and 0.2%40 ten thousand molecular weight chitosans mixture, then sedimentation separation 70min, i.e.,
Light yellow and transparent synanthrin scavenging solution is obtained, uses the measurement of K9805 type kjeldahl apparatus with the impurity removal percentage of proteinometer
It is 88.5%；Corn stalk powder is added into isolated precipitating flocculate, filtration drying, which is made needed for Feed Manufacturing, matches
Material.
Claims (10)
1. a kind of purification process of synanthrin extracting solution, it is characterised in that the step of purification process is as follows:
A, it alkalizes
Alkaline earth oxide or alkaline earth metal hydroxide are added into synanthrin extracting solution, make the pH value of the synanthrin extracting solution
Reach 10.0 or more, 10~40min of quaternization is then carried out under conditions of 30~65 DEG C of temperature, obtains a kind of alkalization synanthrin
Extracting solution
B, phosphoric acid is handled
Under conditions of 65~100 DEG C of temperature, phosphoric acid is added into the alkalization synanthrin extracting solution that step A is obtained mentions alkalization synanthrin
It takes the pH value of liquid to reach 6~8, then carries out 15~40min of neutralization reaction, obtain a kind of neutralization synanthrin extracting solution；
C, it is separated by solid-liquid separation
It sends the neutralization synanthrin extracting solution that step B is obtained in liquid-solid settlement separator, while the past neutralization synanthrin extracting solution
Whether middle addition flocculant or not, after mixing 20~90min of sedimentation separation, the synanthrin solution purified.
2. purification process according to claim 1, it is characterised in that in step, the alkaline earth oxide is
Calcium oxide or magnesia；The alkaline earth metal hydroxide is calcium hydroxide or magnesium hydroxide.
3. purification process according to claim 1, it is characterised in that in step, the pH value of the synanthrin extracting solution reaches
To 10.0~12.0.
4. purification process according to claim 1, it is characterised in that in stepb, the concentration of the phosphoric acid is with weight
Meter 5~75%.
5. purification process according to claim 1, it is characterised in that in stepb, can be added while adding phosphoric acid
Inorganic acid or organic acid；The inorganic acid is sulfuric acid, sulfurous acid or boric acid；The organic acid is acetic acid, propionic acid, citric acid
Or oxalic acid.
6. purification process according to claim 5, it is characterised in that in stepb, phosphoric acid and inorganic acid or organic acid
Molar ratio is 1:1~9.
7. purification process according to claim 1, it is characterised in that in step C, the flocculant is a kind of or more
Kind is selected from aluminium polychloride, aluminum chloride hydrocarbon complex, aluminium polychloride, zinc polysilicate, bodied ferric sulfate, polyacrylamide or shell
The flocculant of glycan.
8. purification process according to claim 1, it is characterised in that in step C, the additive amount of the flocculant be with
Neutralize synanthrin extracting solution poidometer 0.001~0.01%.
9. purification process according to claim 1, it is characterised in that in step C, the precipitating that sedimentation separation obtains is flocculated
Object is directly used in forage compounding or organic fertilizer raw material.
10. purification process according to claim 1, it is characterised in that in step C, the precipitating that sedimentation separation obtains is flocculated
Object is used for forage compounding or organic fertilizer raw material after filtration and or drying.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111111256A (en) * | 2020-01-06 | 2020-05-08 | 江苏泽博环保科技有限公司 | Method and device for purifying plant water extracting solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5865899A (en) * | 1993-07-19 | 1999-02-02 | Applexion | Process for refining a raw sugar, particulary raw sugar from the sugar cane sugar industry |
| CN104059158A (en) * | 2014-06-17 | 2014-09-24 | 熊鹏 | Leaching method of alantin |
| CN106632523A (en) * | 2016-12-12 | 2017-05-10 | 广西轻工业科学技术研究院 | Purification method of D-arabinose |
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2018
- 2018-07-24 CN CN201810816434.7A patent/CN108929391A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5865899A (en) * | 1993-07-19 | 1999-02-02 | Applexion | Process for refining a raw sugar, particulary raw sugar from the sugar cane sugar industry |
| CN104059158A (en) * | 2014-06-17 | 2014-09-24 | 熊鹏 | Leaching method of alantin |
| CN106632523A (en) * | 2016-12-12 | 2017-05-10 | 广西轻工业科学技术研究院 | Purification method of D-arabinose |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111256A (en) * | 2020-01-06 | 2020-05-08 | 江苏泽博环保科技有限公司 | Method and device for purifying plant water extracting solution |
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