CN1281158C - Extraction of water soluble organic calcium from egg shell of birds and preparation of two-calcium nutrient intensifying liguor - Google Patents
Extraction of water soluble organic calcium from egg shell of birds and preparation of two-calcium nutrient intensifying liguor Download PDFInfo
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- CN1281158C CN1281158C CNB031173403A CN03117340A CN1281158C CN 1281158 C CN1281158 C CN 1281158C CN B031173403 A CNB031173403 A CN B031173403A CN 03117340 A CN03117340 A CN 03117340A CN 1281158 C CN1281158 C CN 1281158C
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Abstract
The present invention discloses a method for extracting water-soluble organic calcium from poultry eggshells. In the method, eggshells are treated by washing, drying, pulverization, calcination, acid hydrolysis, acid washing, impurity removal, drying and micronization to obtain the finished product. The present invention also discloses two calcium nutrition fortified agents compounded by the extracted water-soluble organic calcium, which are prepared by mixing dissolution, glue milling emulsification and drying micronization and can be applied to fruit beverages and table vinegar brewing for nutrition fortification.
Description
Technical field
The invention relates to the extracting method of water-soluble organic calcium, and the compound method of two kinds of calcium-nutrition intensifying agents.More particularly, the invention relates to the birds, beasts and eggs shell and extract water-soluble organic calcium, and the compound method of preparing two kinds of calcium-nutrition intensifying agents with the water-soluble organic calcium that extracts.
Background technology
At present, in the Creta Preparata of selling on the market, manyly be water dissolving calcium and contain strong basicity not, though after acid treatment still the stomach to the people excitant is arranged; And the calcium-nutrition intensifying agent that is used to contain acid beverage or making vinegar yet there are no sale." food science and technology " magazine calendar year 2001 2 interim " selection of best shell membrane release agent and preparations of organic calcium " literary composition once carried out report to prepare organic calcium with egg shell, but did not extract the detailed description of water-soluble organic calcium or above-mentioned calcium-nutrition intensifying agent compounding method.
Summary of the invention
The present invention be overcome more existing calcium agent water insoluble or the band strong basicity (acidity) shortcoming, a kind of easy production technology is disclosed, from the birds, beasts and eggs shell, extract a kind of good water solubility, the biological organic calcium hardening agent that does not have the cheapness of any alkali (acid) property can be widely used in the calcium-nutrition intensifying of various foods (medicine) product.And contain the shortcoming that acid solution body food easily makes calcium precipitate at some, and make two kinds of calcium-nutrition intensifying agents, can be used for making vinegar, the calcium-nutrition intensifying of fruit drink.
The present invention is achieved by following proposal: clean the birds, beasts and eggs shell, wash (1), removes impurity, is crushed to the powder of 250～150 μ m after drying; (2) egg-shell meal is become white or pale powder with 850 ℃～1000 ℃ high-temperature calcinations; (3) edible ice acetic acid is standby with the hydrotropy liquid that sterile purified water is mixed with acetic acid content 30%～45%; (4) with hydrotropy liquid with the calcining egg-shell meal in 3.5～7: 1 ratio was mixed hydrotropy 21～30 hours; (5) calcium solution hydrotropy finished is washed acid with the sterile purified water dilution that is equivalent to 3～4 times of solution amount, and staticly settles and get the dry disacidify of supernatant after 2～4 hours; (6) gained calcium powder behind the dry disacidify is used again the sterile purified water with preceding same amount washed, dissolve, staticly settle 5-10 hour, remove the floating foam of solution surface with the screen net during this time, after treating contamination precipitation, it is dry or with after other method drying with the high-pressure spray-drying machine to get supernatant, gets product to 180～120 μ m with micropowder grinding is fine.
The gained calcium powder be will extract again and carrier reinforcement required dosage and propylene glycol alginate pressed, the food-grade xanthans carry out composite after, give be mixed even, according to material require with after the sterile purified water dissolving, grind two times with colloid mill glue, the calcium composite solution, again with solution with 50 ℃～70 ℃ low temperature drying after, finely promptly get calcium-nutrition intensifying agent to 180～120 μ m.
Preferably 900 ℃～950 ℃ of the calcining heats of described birds, beasts and eggs shell; Described egg-shell meal preferably is sintered into white; The acetic acid content of described hydrotropy liquid is preferably 35%～40%; Described hydrotropy liquid is preferably 5～6 with the proportioning of calcining egg-shell meal: 1; The described hydrotropy time is preferably 24～28 hours; The baking temperature of the calcium composite solution that described calcium powder+propylene glycol alginate+xanthans is prepared is preferably 50 ℃～60 ℃.
The specific embodiment
The invention will be further described below in conjunction with embodiment.
(1) the birds, beasts and eggs shell is cleaned, washes, removes stain, impurity.(2) with the powder of birds, beasts and eggs shell crushed after being dried to 250～150 μ m of cleaning up.(3) egg-shell meal is become white or pale powder with 850 ℃～1000 ℃ high-temperature calcination; The best calcining degree of egg-shell meal is for being sintered into white powder.(4) edible ice acetic acid is standby with the acetic acid hydrotropy liquid that sterile purified water is mixed with acetic acid content 30%～45%, acetic acid content the best of hydrotropy liquid is 35%～40%.(5) with hydrotropy liquid and egg-shell meal in 3.5～7: 1 ratio proportioning, the best proportioning of hydrotropy liquid and egg-shell meal is 5～6: 1.(6) the acetic acid hydrotropy liquid of proportioning is packed into earlier stainless steel in pottery or the food grade plastic container, is poured the egg-shell meal of proportioning into container again, and constantly stirs, and it is fully mixed, and question response slows down and stops back covered container lid.(7) the association reaction time of egg-shell meal and hydrotropy liquid is 21～30 hours, during should stir mixed 2～3 times, the hydrotropy time was the best with 24～28 hours.(8) dissolve the egg-shell meal of finishing and form a kind of acid calcium solution, wash acid with the sterile purified water dilution that is equivalent to 3～4 times of calcium solutions again, and after staticly settling 2～4 hours, it is standby to get supernatant.(9) with the supernatant obtained with 95 ℃～110 ℃ high temperature drying disacidifies, the disacidify calcium powder.(10) the gained calcium powder is used and the washing of the sterile purified water of preceding same amount, stirring and dissolving again, after dissolving finishes, was staticly settled 5-10 hour, and remove the floating foam of solution surface with the screen net, treat contamination precipitation after, it is standby to get supernatant.(11) supernatant obtained is promptly got product with micropowder grinding is fine to 180～120 μ m with the high-pressure spray-drying machine after dry or other method drying.
To extract water-soluble organic calcium powder and propylene glycol alginate, the food-grade xanthans of gained again and make following proportioning:
(1) is used for the calcium-nutrition intensifying that fruit drink etc. contains the liquid food of acid.
100ml fruit juice proportioning 50～200mg calcium powder+25～50mg propylene glycol alginate+25～50mg xanthans.
(2) be used for the calcium-nutrition intensifying of making vinegar.
100ml making vinegar proportioning 50～2000mg calcium powder+50mg propylene glycol alginate+150mg xanthans or 150mg propylene glycol alginate+50mg xanthans.
To strengthen the good calcium powder of dosage ratio according to carrier earlier, propylene glycol alginate, xanthans give be mixed even after, with sterile purified water dilution dissolving,, make that it fully mixes, emulsification according to material require again with colloid mill glue mill two times, uniform calcium composite solution.With gained solution with 50 ℃～70 ℃ low temperature drying after, get product to 180～120 μ m with micropowder grinding is fine.The optimum temperature of low temperature drying is 50 ℃～60 ℃.
Be the specific embodiment that from the birds, beasts and eggs shell, extracts water-soluble organic calcium below, and the preparation example of two kinds of calcium-nutrition intensifying agents.Can further understand best proportioning, the recovery rate that from the birds, beasts and eggs shell, extracts water-soluble organic calcium by the contrast of specific embodiment, and the difference reinforcement dosage and the material mixture ratio amount that are used for two kinds of liquid food calcium-nutrition intensifyings.
Example 1: calcining egg shell powder 10g, acetic acid content 30% hydrotropy liquid 35ml, hydrotropy got calcium lysate 35ml in 23 hours, wash acid with sterile purified water 100ml dilution, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 2 hours, use the washing of 120ml sterile purified water, dissolving, removal of impurities again, staticly settled 5 hours and removed solution surface with the screen net and float foam, get the dry finished product that gets of supernatant.
Example 2: calcining egg shell powder 10g, acetic acid content 40% hydrotropy liquid 40ml, hydrotropy got calcium lysate 35ml in 23 hours, add sterile purified water 140ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 2 hours, again with the washing of 140ml sterile purified water, the dissolving removal of impurities, staticly settled 8 hours and removed solution surface with the screen net and float foam, get the dry finished product that gets of supernatant.
Example 3: calcining egg shell powder 10g, acetic acid content 45% hydrotropy liquid 40ml, hydrotropy got calcium lysate 40ml in 23 hours, add sterile purified water 140ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 2 hours, again with the washing of 140ml sterile purified water, the dissolving removal of impurities, staticly settled 8 hours and removed solution surface with the screen net and float foam, get the dry finished product that gets of supernatant.
Example 4: calcining egg shell powder 10g, acetic acid content 35% hydrotropy liquid 35ml, hydrotropy got calcium lysate 40ml in 22 hours, add sterile purified water 130ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 2 hours, again with the washing of 150ml sterile purified water, the dissolving removal of impurities, staticly settled 10 hours and removed solution surface with the screen net and float foam, get the dry finished product that gets of supernatant.
Example 5: calcining egg shell powder 10g, acetic acid content 37% hydrotropy liquid 50ml, hydrotropy got calcium lysate 50ml in 24 hours, add sterile purified water 150ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 2 hours, with the washing of 150ml sterile purified water, dissolving removal of impurities, staticly settled 10 hours and removed solution surface with the screen net and float foam again, get the dry finished product that gets of supernatant.
Example 6: calcining Ovum Anas domestica putamina powder 9150mg, acetic acid content 37% hydrotropy liquid 55ml, hydrotropy got calcium lysate 50ml in 28 hours, add sterile purified water 200ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 4 hours, again with the washing of 200ml sterile purified water, the dissolving removal of impurities, staticly settled 10 hours and remove the floating foam of solution surface with the screen net, get after the supernatant drying finished product.
Example 7: calcining Ovum Anas domestica putamina powder 9150mg, acetic acid content 40% hydrotropy liquid 58ml, hydrotropy 21 hours 30 minutes calcium lysate 55ml, add sterile purified water 160ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 4 hours, again with the washing of 200ml sterile purified water, the dissolving removal of impurities, staticly settled 5 hours and remove the floating foam of solution surface with the screen net, get after the supernatant drying finished product.
Example 8: calcining goose egg-shell powder 3400mg, acetic acid content 37% hydrotropy liquid 25ml, hydrotropy got calcium lysate 22ml in 22 hours, add sterile purified water 70ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 3 hours, again with the washing of 100ml sterile purified water, dissolving removal of impurities, staticly settled 5 hours and remove the floating foam of solution surface with the screen net, get after the supernatant drying finished product.
Example 9: calcining goose egg-shell powder 3400mg, acetic acid content 40% hydrotropy liquid 25ml, hydrotropy 21 hours 30 minutes calcium lysate 20ml, add sterile purified water 60ml dilution and wash acid, staticly settle and got dry disacidify (alkali) calcium powder that gets of supernatant in 2 hours, again with the washing of 100ml sterile purified water, dissolving removal of impurities, staticly settled 5 hours and remove the floating foam of solution surface with the screen net, get after the supernatant drying finished product.
With the water-soluble organic calcium that above-mentioned example extracts, strengthen the dosage difference according to carrier, respectively with propylene glycol alginate, after the xanthans proportioning, make the hardening agent that is used for fruit drink, making vinegar calcium-nutrition intensifying.
Be the specific embodiment of two kinds of calcium-nutrition intensifying agents below:
Example 1:(1) 100ml fruit juice proportioning 50mg calcium powder+25mg propylene glycol alginate+25mg xanthans, (2) 100ml fruit juice proportioning 100～200mg calcium powder+50mg propylene glycol alginate+50mg xanthans.
The calcium-nutrition intensifying agent of producing with said ratio add advance in the fruit juice after, except that the suitable concentration that improves fruit juice, impression is all identical with original fruit juice on the eating mouth feel outside, checks not have the generation of precipitation in 30 days through leaving standstill to deposit.
Example 2:(1) 100ml making vinegar proportioning 50～150mg calcium powder+50mg propylene glycol alginate+100mg xanthans, (2) 100ml making vinegar proportioning 200～2000mg calcium powder+50mg propylene glycol alginate+150mg xanthans or 150mg propylene glycol alginate+50mg xanthans.
With the calcium-nutrition intensifying agent that said ratio is produced, all identical on the eating mouth feel at colourity, vinegar fragrance except that the concentration of suitable raising making vinegar after interpolation is advanced in the making vinegar with former vinegar, checked through leaving standstill to deposit that deposit-free produced in 60 days.
Claims (7)
1, a kind of method of extracting water-soluble organic calcium from the birds, beasts and eggs shell is characterized in that, it comprises the following steps: that (1) clean the birds, beasts and eggs shell washing; (2) will wash clean egg shell crushed after being dried to 250～150 μ m powder; (3) egg-shell meal is become white or pale powder with 850～1000 ℃ of high-temperature calcinations; (4) edible ice acetic acid is standby with the acetic acid hydrotropy liquid that sterile purified water is mixed with acetic acid content 30%～45%; (5) acetic acid hydrotropy liquid and calcining is ripe egg-shell meal is in 3.5～7: 1 ratio proportioning; (6) in acetic acid hydrotropy liquid that proportioning is good is packed stainless steel, pottery or food grade plastic container earlier into, pour the calcining egg-shell meal of proportioning into container again, and constantly stir, the question response back covered container lid that slows down; (7) egg-shell meal is 21～30 hours with the hydrotropy time that combines of hydrotropy liquid, during should stir mixed 2～3 times; (8) calcium solution that hydrotropy finished is washed acid with the sterile purified water dilution that is equivalent to 3～4 times of solution amount, staticly settle 2～4 hours after, it is standby to get supernatant; (9) with the supernatant obtained with 95 ℃～110 ℃ high temperature drying disacidify after, the disacidify calcium powder; (10) the gained calcium powder is used and sterile purified water washing, the dissolving of (8) same amount, treat that the calcium powder dissolving finishes after, staticly settled 5～10 hours, remove the floating foam of solution surface with the screen net, treat contamination precipitation after, it is standby to get supernatant; (11) dry or other method gets product to 180～120 μ m with micropowder grinding is fine in dry back with the high-pressure spray-drying machine with the supernatant obtained.
2, the extracting method of water-soluble organic calcium according to claim 1 is characterized in that, the high-temperature calcination that described egg-shell meal application is 900 ℃～950 ℃ becomes white powder.
3, the extracting method of water-soluble organic calcium according to claim 1 is characterized in that, the acetic acid content of described hydrotropy liquid is 35%～40%; Described hydrotropy liquid is 5～6: 1 with the proportional quantity of calcining egg-shell meal; 24～28 hours described hydrotropy time.
4, the extracting method of water-soluble organic calcium according to claim 1 is characterized in that, described calcium lysate is used the sterile purified water dilution that is equivalent to 4 times of solution amount and washed acid; Staticly settle and get the dry disacidify of supernatant after 3～4 hours; Described calcium powder is used sterile purified water washing, dissolving, the removal of impurity with preceding same amount, and leaves standstill and get after 6～8 hours that supernatant is dry finely to get product to 150 μ m.
5, a kind of production technology of preparing calcium-nutrition intensifying agent is characterized in that, will make following proportioning according to water-soluble organic calcium and propylene glycol alginate, food-grade xanthans that the described method of claim 1 makes:
With 100ml fruit juice is the carrier proportioning
Calcium powder 50～200mg propylene glycol alginate 25～50mg xanthans 25～50mg
With above-mentioned three kinds of materials respectively by described dosage ratio, and give be mixed even after, with the sterile purified water dissolving, send colloid mill glue mill two times, the calcium composite solution, use 50 ℃～70 ℃ low temperature dryings again after, finely get product to 180～120 μ m.
6, a kind of production technology of preparing calcium-nutrition intensifying agent is characterized in that, will make following proportioning according to water-soluble organic calcium and propylene glycol alginate, food-grade xanthans that the described method of claim 1 makes:
With the 100ml making vinegar is the carrier proportioning
Calcium powder 50～2000mg propylene glycol alginate 50mg xanthans 150mg
With above-mentioned three kinds of materials respectively by described dosage ratio, and give be mixed even after, with the sterile purified water dissolving, send colloid mill glue mill two times, the calcium composite solution, use 50 ℃～70 ℃ low temperature dryings again after, finely get product to 180～120 μ m.
7, a kind of production technology of preparing calcium-nutrition intensifying agent is characterized in that, will make following proportioning according to water-soluble organic calcium and propylene glycol alginate, food-grade xanthans that the described method of claim 1 makes:
With the 100ml making vinegar is the carrier proportioning
Calcium powder 50～2000mg propylene glycol alginate 150mg xanthans 50mg
With above-mentioned three kinds of materials respectively by described dosage ratio, and give be mixed even after, with the sterile purified water dissolving, send colloid mill glue mill two times, the calcium composite solution, use 50 ℃～70 ℃ low temperature dryings again after, finely get product to 180～120 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB031173403A CN1281158C (en) | 2003-02-25 | 2003-02-25 | Extraction of water soluble organic calcium from egg shell of birds and preparation of two-calcium nutrient intensifying liguor |
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| CNB031173403A CN1281158C (en) | 2003-02-25 | 2003-02-25 | Extraction of water soluble organic calcium from egg shell of birds and preparation of two-calcium nutrient intensifying liguor |
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| CN101273779B (en) * | 2008-05-12 | 2011-11-16 | 吉林大学 | Method for preparing food products with high osteocalcin |
| CN102524521B (en) * | 2012-02-29 | 2014-01-08 | 重庆市畜牧科学院 | Preparation method of eggshell hydrolysate, as well as product and application of eggshell hydrolysate |
| CN103238643B (en) * | 2012-09-24 | 2014-09-24 | 河北同和生物制品有限公司 | Biological calcium supplement special for flour |
| CN103892285B (en) * | 2014-04-10 | 2015-08-19 | 青岛食安生物工程有限公司 | The preparation technology of pure natural ultra micro calcium powder |
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