CN1294128A

CN1294128A - Process for preparing phytic acid

Info

Publication number: CN1294128A
Application number: CN 00123173
Authority: CN
Inventors: 李国荣
Original assignee: Individual
Current assignee: Individual
Priority date: 2000-10-30
Filing date: 2000-10-30
Publication date: 2001-05-09
Anticipated expiration: 2020-10-30
Also published as: CN1107071C

Abstract

A process for preparing phytic acid includes crushing bran cake, sieving by 40 meshes to obtain rice bran, adding ionic water at 60 deg.C to hyrochloric acid slowly to regulate pH value to 2.0, mixing with bran with water in weight ratio of 1:8, immersing for 4-6 hr while stirring at intervals of 30 min, laying aside for 2 hr, getting supernatant, adding water to the dregs, regulating pH to 2.0, immersing for 2 hrs, laying aside for 1 hr, getting supernatant, merging said supernatant, filter to obtain mother liquid, washing, acidifying exchange, and concentrating.

Description

A kind of producing and manufacturing technique of phytic acid

The present invention relates to a kind of production method of phytic acid.

Phytic acid is a myo-Inositol hexaphosphate, extensively is present in the oil grain, particularly presses oily grouts, more as content in rice bran cake, soya-bean cake, rapeseed cake, linseed meal, cotton seed cake, wheat bran, wheat bran, the maize germ.The phytic acid of occurring in nature does not exist with free form, but exists with the form of phytic acid ca (luxuriant and rich with fragrance fourth).Phytic acid is faint yellow or isabelline thickness body, is strongly-acid, and is soluble in water.The feature of phytic acid is with metal ion extremely strong complex ability and oxidation-resistance to be arranged; complexing power is similar to EDTA; and belong to the safety non-toxic natural nutriment; in developed country; phytic acid has been widely used in industries such as food, medicine, chemical industry; in wine manufacturing industry, the adding phytic acid can be removed Ca, Fe, Cu and other metallic element in the wine, and the protection HUMAN HEALTH is had good action.Phytic acid also can be used as the preservation agent of fishery products, fruit and vegetable, flowers, the tinned pre-colour-protecting stabilizing agent, and fatty foods, meat, cake, the anticorrosion preservatives of salad, beverage remove metal agent.In fermentative Production lactic acid, riboflavin, gentamicin, the antibiotic process of amino glycoside, add phytic acid and can improve output.Pharmaceutically, can make oxidation inhibitor, also can be used as therapeutical agent, the artificial tooth cleaning agent of scanning imagery agent, gastritis and enteritis.The production method of phytic acid is a lot of at present, as calcium Fei Dingfa, ammonia Fei Dingfa, Na Feidingfa etc.Wherein, Na Feidingfa produces the comparatively reliable and advanced method of phytic acid.But also have weak point, its main drawback has:

1, to adopt tap water to soak, contain the extraction yield of metal ion, phytic acid low for this kind method, has only 7-10%.

2, be provided with anion column and sulfate radical, the residues of chloride amount is big, reaches 3-5%, influences quality.

Purpose of the present invention provides the phytic acid production technique that a kind of phytic acid content height, inorganic phosphorus do not exceed standard.

The producing and manufacturing technique of phytic acid of the present invention is:

1, acidleach

The chaff cake was pulverized 40 mesh sieves, and it is standby to make rice bran.60 ℃ ionized waters are slowly added hydrochloric acid, pH value is transferred to 2.0, add the rice bran of preparation then, the weight ratio of rice bran and water is 1: 8.Rice bran soaked 4-6 hour, stirred once in per 30 minutes, after stirring, also will survey pH value, and remaining on pH value is 2.0, inaccessiblely will add hydrochloric acid.After leaving standstill two hours like this, extract supernatant liquid.

Secondary soaks, and adds water by 1: 4 in sediment, water temperature 60 degree, pH value is transferred to 2.0, stirs once every 30 minutes, soaks two hours, leave standstill one hour after, the extraction supernatant liquid.

2, merge

The secondary supernatant liquor merges, and it should be as clear as crystal filtering the mother liquor that flows out.Mother liquor is opaque, filters again, till as clear as crystal.

3, neutralization

Transparent mother liquor neutralizes with alkali.With solid sodium hydroxide, use a spot of water dissolution, Yi Bian slowly add in the mother liquor, stir on one side, approximately the 100kg mother liquor restrains sodium hydroxide with 200-250, adds after the alkali, transparent mother liquor has become oyster white, and surveying pH value with test paper is 8, just stops to add sodium hydroxide.Fei Ting just precipitates after adding alkali reaction.If it is too much that sodium hydroxide adds, luxuriant and rich with fragrance spit of fland is fully precipitated, but color burn causes the washing difficulty; If the sodium hydroxide dosage is not enough, can not fully react, the precipitation capacity of phytic acid composition is just few.In and the time add how much sodium hydroxide, specifically be to decide with pH value.After the neutralization reaction, staticly settled two hours, then yellow waste water is taken out, extract the luxuriant and rich with fragrance spit of fland of lower sediment thing.

4, washing

The luxuriant and rich with fragrance spit of fland of precipitation is placed in the Da Chi, and pH value is transferred to 8.Fei Ting wants complete dissolved particles just can touch water, just can reach the purpose of washing, dissolves later Fei Ting and is placed on centrifuge dehydration on the whizzer, repetitive scrubbing three times.

5, wash with pure water

After repeatedly sodium hydroxide washs, wash with pure water again.Luxuriant and rich with fragrance spit of fland stirring and dissolving (water no longer adds any medicine) in water is washed neutrality to luxuriant and rich with fragrance spit of fland to be as the criterion.During the pure water washing, at first measure the pure water pH value,, just wash 6.5 if the pure water pH value is 6.5; The pH value of water is 7.0 just to wash 7.0.After the pure water washing, centrifuge dehydration.

6, acidifying

732 types handled well sun resin, washing pH value with pure water is 3.5-4, behind the filter solid carbon dioxide, by the i.e. two parts of luxuriant and rich with fragrance spits of fland of resins portion of 2: 1 ratios, puts resin earlier into, after put Fei Ting.Fei Ting runs into resin and becomes liquid with regard to dissolving, and should be 1.5 with precision test paper test PH this moment, is the best pH-value of acidifying.If basicity is higher, increase resin, basicity is on the low side, adds luxuriant and rich with fragrance spit of fland.Dissolving is static two hours in basin, with cloth bag resin filter is separated then, and filtrate also is acidizing fluid.

7, exchange

Positive resin after the manipulation of regeneration installs to exchange king-post the inside together with the salt sour water.6 centimeters of king-post internal diameters, long 1.2 meters, 3 is positive post, same two is cloudy post.Use the resin drip washing in the pure water coupled columns then, the water that flows out, pH value reaches 3.5-4, stops drip washing, the current for the treatment of bottom in the post in after just can feed acidizing fluid, the control flow velocity is at per minute 50-60 milliliter.The exchange that enters two cloudy king-posts again after the exchange of three posts is intact so just draws purer rare value acid.

8, concentrate

Rare value acid solution is poured in the evaporation tank, and concentrated degree Beaume is 12 when spending, and carries out the decolouring first time, under temperature at that time, add 1% activated carbon, after stirring, use the middling speed filter paper filtering, the black active carbon filtration is come out, the phytic acid that leaches carries out concentrating the second time, temperature is controlled at below 60 ℃, when degree Beaume reaches 41-43, carries out the decolouring second time, add activated carbon 1% equally, use the middling speed filter paper filtering equally, effusive should be transparent white or weak yellow liquid, and this liquid is the phytic acid finished product.

The present invention has been owing to adopted the novel process of acidleach, thereby improved the content and the extraction yield of phytic acid greatly, removed metal ion simultaneously.The present invention is by making pure milky phytic acid with novel process in the alkali.Particularly adopt novel concentrating process of the present invention to pass through secondary concentration, temperature is controlled at below 60 ℃, and the pure milky phytic acid of producing has kept the pure natural true qualities, has reduced muriatic residual quantity, and the content that can make inorganic phosphorus reaches the specified standards requirement, improved the quality of phytic acid.

Embodiment

The chaff cake was pulverized 40 mesh sieves, and to make the 1kg rice bran standby.The ionized water of 60 ℃ of 8kg is slowly added hydrochloric acid, pH value is transferred to 2.0, add the 1kg rice bran of preparation then, soaked 5 hours, stirred once every 30 minutes, and inspection side pH value, PH does not reach 2.0 and adds the small amount of hydrochloric acid adjusting again, reaches till 2.0 up to pH value.Soak after 5 hours, left standstill again 2 hours, extract supernatant liquid then.Secondary soaks, and adds 4kg water in sediment, and water temperature is 60 ℃, and pH value is transferred to 2.0, stirs once every 30 minutes, soaks 2 hours, leaves standstill after 1 hour and extracts supernatant liquid.The supernatant liquid of second decimation is merged, and be filled into infuse clearly transparent till.The transparent mother liquor of infusing clearly that filters out closes in carrying out with alkali, solid-state sodium hydroxide with the less water dissolving after, slowly add in the mother liquor on one side, stirring on one side, pH value is transferred at 8 o'clock, stop adding sodium hydroxide.This moment, milky luxuriant and rich with fragrance spit of fland was fully precipitated.Leave standstill after two hours yellow waste water is taken out, the luxuriant and rich with fragrance spit of fland of the lower sediment thing that extracts is placed on and uses pure cerium hydroxide sodium repetitive scrubbing three times in the Da Chi, and use centrifuge dewatering, wash with pure water again, neutrality is washed in luxuriant and rich with fragrance spit of fland to be as the criterion, centrifuge dehydration is put into the 732 types sun resin of handling well and is carried out acidifying, and the luxuriant and rich with fragrance spit of fland that will become liquid is fully stirred and made pH value reach 1.5.Leave standstill after two hours and with cloth bag resin filter is separated, filtrate is that acidizing fluid is stand-by.Positive resin after handling and salt sour water are installed to exchange king-post the inside together.With pure water the resin in the king-post is carried out drip washing then, the pH value of the water that flows out reaches at 3.5 o'clock and stops drip washing, just can feed acidizing fluid after the current for the treatment of bottom in the post are done.Through entering two positive king-post exchanges after three positive post exchanges again, just can obtain purer thin planting acid.Dilute phytic acid solution poured in the evaporation tank concentrate, when concentrating degree Beaume 12 and spending, carry out decolouring first time, add 1% activated carbon, stir, use the middling speed filter paper filtering, the black active carbon filtration is come out, and the phytic acid that leaches carries out concentrating the second time, and temperature is controlled at below 60 ℃.When degree Beaume reaches 41-43, carry out the decolouring second time, add activated carbon 1% equally, filter with the middling speed filter paper at last and just make the phytic acid finished product.

Claims

1, a kind of producing and manufacturing technique of phytic acid is characterized in that:

A, the chaff cake was pulverized 40 mesh sieves, and to make rice bran standby, and 60 ℃ ionized waters are slowly added hydrochloric acid, and pH value is transferred to 2.0, add the rice bran of preparation then, the weight ratio of rice bran and water is 1: 8, soaks 4-6 hour, stirred once every 30 minutes, leave standstill after two hours and extract supernatant liquid;

B, secondary soak, and in sediment, add water by 1: 4, and water temperature is 60 ℃, and pH value is transferred to 2.0, stir once every 30 minutes, soak two hours, leave standstill one hour after, the extraction supernatant liquid; The supernatant liquid of second decimation is merged, through filtering, obtain transparent mother liquor again;

C, transparent mother liquor neutralize with alkali.The a spot of water dissolution of pure cerium hydroxide sodium slowly adds in the mother liquor, and pH value is transferred at 8 o'clock, stops hydro-oxidation sodium, after the neutralization reaction, staticly settles two hours, extracts the luxuriant and rich with fragrance spit of fland of lower sediment thing;

D, first with washing with pure water again after the soda ash washing, then with centrifuge dehydration sedimentary phytic acid;

Acidifying is carried out with the 732 types sun resin of handling well in luxuriant and rich with fragrance spit of fland after E, the washing, it is 3.5-4 that 732 types sun resin washes pH value with water, after the filter solid carbon dioxide divides, mix with luxuriant and rich with fragrance spit of fland in 2: 1 ratios, best pH value after the acidifying is 1.5, with cloth bag resin and acidizing fluid are separated then, acidizing fluid obtains thin planting acid after the exchange column exchange;

F, rare value acid solution is poured in the evaporation tank, when concentrated degree Beaume is 12 ℃, carried out the decolouring first time, add 1% activated carbon, after stirring, use the middling speed filter paper filtering, the black active carbon filtration is come out, filtrate carries out concentrating the second time, and temperature is controlled at below 60 ℃, when degree Beaume reaches 41-43, carry out the decolouring second time, and add 1% activated carbon equally, and use the middling speed filter paper filtering again, just can be made into the phytic acid finished product.