CN102887823A - Method for preparing calcium lactate by eggshell vacuum neutralization - Google Patents
Method for preparing calcium lactate by eggshell vacuum neutralization Download PDFInfo
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- CN102887823A CN102887823A CN2012104079282A CN201210407928A CN102887823A CN 102887823 A CN102887823 A CN 102887823A CN 2012104079282 A CN2012104079282 A CN 2012104079282A CN 201210407928 A CN201210407928 A CN 201210407928A CN 102887823 A CN102887823 A CN 102887823A
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Abstract
The invention relates to a method for preparing calcium lactate by eggshell vacuum neutralization. The method comprises the following steps: rolling eggshells, carrying out rough grinding to promote shell membrane separation, rinsing with running water, removing residual egg white and shell membrane, baking at 100-130 DEG C, drying at 80 DEG C, and screening to remove sand; carrying out fine grinding to 60 meshes, 100 meshes, 200 meshes or 300 meshes to obtain eggshell powder; mixing lactic acid and excessive stoichiometric eggshell powder to react under the vacuum degree of 0.01-0.08 Mpa at 30-55 DEG C, and carrying out vacuum filtration after the reaction finishes, wherein the filtrate is for later use, and the concentration of the lactic acid is 5-20%; concentrating the filtrate under reduced pressure to 50-70 vol%, refrigerating in a 5 DEG C refrigerator for 4 hours, and carrying out vacuum filtration to obtain calcium lactate coarse crystals; and eluting the calcium lactate coarse crystals with absolute ethanol for 40 minutes three times, carrying out vacuum filtration, and drying at 80 DEG C to obtain the calcium lactate of which the purity is up to 98%, wherein the solid-liquid volume ratio for elution is 1:2-1:6.
Description
Technical field
The invention belongs to livestock and poultry by product processing and utilization field, particularly prepare the method for calcium lactate with eggshell.
Background technology
China supports the maximum country of fowl in the world, continuous 20 years the first in the world of egg productivity.The bright egg total amount of China in 2007 reaches 3.1xl0
10About kg.Eggshell accounts for 11% ~ 13% of bright egg size amount, accounts for 12% of egg size by eggshell and calculates, and China produces more than 400 ten thousand tons of eggshells every year.Eggshell is thrown into scrap heap in batches, not only to environment, also is the waste of resource.If eggshell is collected, fully utilize, both increased economic benefit, avoid again the pollution to environment, thereby strengthened the development and use to eggshell resource, have huge economic implications and social effect.
Because the calcium in the eggshell is CaCO more than 90%
3Be inorganic precipitation calcium, be difficult in vivo digested absorption, can not be directly used in food, the fodder production.Therefore, for improving the specific absorption of calcium in the eggshell, usually inorganic calcium to be converted into organic calcium, could be absorbed well and utilize.At present calcium carbonate transforms the method for producing organic calcium and mainly contains in the eggshell: high-temperature calcination, directly neutralisation, microbe transformation method and raw material soaking method.These four kinds of methods cut both ways, and yet there are no report about the method for preparing calcium lactate that directly neutralizes under the eggshell vacuum environment at present.
Summary of the invention
The object of the invention is intended to prepare the problems such as calcium lactate method yield is not high for existing eggshell, and providing directly neutralizes under a kind of eggshell vacuum environment prepares the method for calcium lactate, reduces the energy consumption in the production process, improves the yield of calcium lactate.
To achieve these goals, technical scheme of the present invention is:
Neutralization prepares the method for calcium lactate under a kind of eggshell vacuum environment, comprises the steps:
(1) preparation of egg-shell meal: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dryings; Sieve, remove gravel; Be finely ground to 60 ~ 300 orders, it is for subsequent use to get egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.01 ~ 0.08Mpa; Lactic acid and egg-shell meal hybrid reaction, egg-shell meal granularity 60 ~ 300 orders, egg-shell meal is by lactic acid and calcium carbonate chemistry reaction formula punishment in advance amount 5% ~ 75%, reaction times 30 ~ 180min, temperature of reaction is 30 ~ 55 ℃, lactic acid concn is 5wt% ~ 20wt%, after question response was finished, with the product suction filtration, reserved filtrate was for subsequent use;
(3) calcium lactate crystallization: the filtrate decompression of step (2) preparation is concentrated into volume percent 50% ~ 70%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in the step (3), wash-out solid-liquid volume ratio is 1:2 ~ 1:6, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactate products that get, product calcium lactate purity reaches 98%.
In above-mentioned preparation method's step (1), be finely ground to 60 orders, 100 orders, 200 orders or 300 orders, it is for subsequent use to get egg-shell meal.
In above-mentioned preparation method's step (1), 100-130 ℃ oven dry 25-30min, 80 ℃ of dry 2h.
Among the above-mentioned preparation method, preferred condition: vacuum tightness 0.04Mpa in the described step (2), egg-shell meal is by lactic acid and calcium carbonate chemistry reaction formula punishment in advance amount 15%, egg-shell meal granularity 100 orders, reaction times 45min, 40 ℃ of temperature of reaction, lactic acid concn is 8.33wt%.
Among the above-mentioned preparation method, preferred condition: described step is concentrated into volume percent 50% with filtrate decompression in (3), places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, and suction filtration gets calcium lactate coarse crystallization body.
Preferred wash-out solid-liquid volume ratio is 1:4 in above-mentioned preparation method's step (4).
With the preparation calcium lactate, adopt above-mentioned each described method to be prepared from the eggshell vacuum.
The invention has the beneficial effects as follows:
Can reduce the energy consumption in the calcium lactate production process, the yield of calcium lactate reaches the quality of 70%(calcium lactate and the mass ratio of egg-shell meal).
Description of drawings
Fig. 1 is the process flow sheet of invention.
Embodiment
Embodiment 1
Neutralization preparation calcium lactate comprises the steps: under the eggshell vacuum environment
(1) preparation of eggshell powder: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dry 2h; Sieve, remove gravel; Be finely ground to 60 orders, 100 orders, 200 orders or 300 orders, it is for subsequent use to get egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.01Mpa; 36g lactic acid solution and egg-shell meal hybrid reaction, egg-shell meal granularity 60 orders, the egg-shell meal amount is by lactic acid and calcium carbonate chemistry reaction formula punishment in advance amount and punishment in advance amount 5%, reaction times 30min, temperature of reaction is 30 ℃, lactic acid concn is after the 20wt% question response is finished, product is filtered, and reserved filtrate is for subsequent use;
(3) calcium lactate crystallization: the filtrate decompression of step (2) preparation is concentrated into volume percent 50%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in the step (3), wash-out solid-liquid volume ratio is 1:2, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactates that get, calcium lactate yield 68%, calcium lactate purity reaches 98%.
Embodiment 2
Neutralization preparation calcium lactate under the eggshell vacuum environment
,Comprise the steps:
(1) preparation of eggshell powder: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dry 2h; Sieve, remove gravel; It is for subsequent use that fine grinding (60 orders, 100 orders, 200 orders, 300 orders) gets egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.03Mpa; 72g lactic acid solution and punishment in advance amount 15% (by lactic acid and calcium carbonate chemistry reaction formula), granularity 100 purpose egg-shell meal hybrid reactions; Reaction times 45min; Temperature of reaction is 40 ℃; After lactic acid concn 12wt% question response was finished, with the product suction filtration, reserved filtrate was for subsequent use;
(3) calcium lactate crystallization: the filtrate decompression of (2) preparation is concentrated into volume percent 60%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in (3), wash-out solid-liquid volume ratio is 1:4, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactates that get, calcium lactate yield 65.93%, calcium lactate purity reaches 98%.
Embodiment 3
Neutralization preparation calcium lactate under the eggshell vacuum environment
,Comprise the steps:
(1) preparation of eggshell powder: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dry 2h; Sieve, remove gravel; It is for subsequent use that fine grinding (60 orders, 100 orders, 200 orders, 300 orders) gets egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.05Mpa; 108g lactic acid solution and punishment in advance amount 35% (by lactic acid and calcium carbonate chemistry reaction formula), granularity 200 purpose egg-shell meal hybrid reactions; Reaction times 80min; Temperature of reaction is 45 ℃; Lactic acid solution concentration is that with the product suction filtration, reserved filtrate was for subsequent use after the 8.33wt% question response was finished;
(3) calcium lactate crystallization: the filtrate decompression of (2) preparation is concentrated into volume percent 70%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in (3), wash-out solid-liquid volume ratio is 1:6, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactates that get, calcium lactate yield 67.90%,, calcium lactate purity reaches 98%.
Embodiment 4
Neutralization preparation calcium lactate under the eggshell vacuum environment
,Comprise the steps:
(1) preparation of eggshell powder: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dry 2h; Sieve, remove gravel; It is for subsequent use that fine grinding (60 orders, 100 orders, 200 orders, 300 orders) gets egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.08Mpa; 144g lactic acid solution and punishment in advance amount 55% (by lactic acid and calcium carbonate chemistry reaction formula), granularity 300 purpose egg-shell meal hybrid reactions; Reaction times 120min; Temperature of reaction is 50 ℃; Lactic acid concn is that with the product suction filtration, reserved filtrate was for subsequent use after the 6.25wt% question response was finished;
(3) calcium lactate crystallization: the filtrate decompression of (2) preparation is concentrated into volume percent 50%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in (3), wash-out solid-liquid volume ratio is 1:4, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactates that get, calcium lactate yield 68.85%,, calcium lactate purity reaches 98%.
Embodiment 5
Neutralization preparation calcium lactate under the eggshell vacuum environment
,Comprise the steps:
(1) preparation of eggshell powder: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dry 2h; Sieve, remove gravel; It is for subsequent use that fine grinding (60 orders, 100 orders, 200 orders, 300 orders) gets egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.08Mpa; 180g lactic acid solution and punishment in advance amount 55% (by lactic acid and calcium carbonate chemistry reaction formula), granularity 300 purpose egg-shell meal hybrid reactions; Reaction times 180min; Temperature of reaction is 55 ℃; The concentration of lactic acid is that with the product suction filtration, reserved filtrate was for subsequent use after the 5wt% question response was finished;
(3) calcium lactate crystallization: the filtrate decompression of (2) preparation is concentrated into volume percent 70%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in (3), wash-out solid-liquid volume ratio is 1:6, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactates that get, calcium lactate yield 60.53%,, calcium lactate purity reaches 98%.
Embodiment 6
Neutralization preparation calcium lactate under the eggshell vacuum environment
,Comprise the steps:
(1) preparation of eggshell powder: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dry 2h; Sieve, remove gravel; It is for subsequent use that fine grinding (60 orders, 100 orders, 200 orders, 300 orders) gets egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.04Mpa; 108g lactic acid solution and punishment in advance amount 15% (by lactic acid and calcium carbonate chemistry reaction formula), granularity 100 purpose egg-shell meal hybrid reactions; Reaction times 30min; Temperature of reaction is 40 ℃; Lactic acid concn is that with the product suction filtration, reserved filtrate was for subsequent use after 8.33% question response was finished;
(3) calcium lactate crystallization: the filtrate decompression of (2) preparation is concentrated into volume percent 50%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in (3), wash-out solid-liquid volume ratio is 1:4, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactates that get, calcium lactate yield 70.08wt%, calcium lactate purity reaches 98%.
Claims (6)
1. neutralization prepares the method for calcium lactate under the eggshell vacuum environment, it is characterized in that comprising the steps:
(1) preparation of egg-shell meal: with the eggshell rolling, corase grind promotes shell membrane to separate; Residue egg white and shell membrane are removed in the flowing water rinsing; 100-130 ℃ oven dry 25-30min; 80 ℃ of dryings; Sieve, remove gravel; Be finely ground to 60 ~ 300 orders, it is for subsequent use to get egg-shell meal;
(2) neutralization preparation calcium lactate under the vacuum environment: at vacuum tightness 0.01 ~ 0.08Mpa; Lactic acid and egg-shell meal hybrid reaction, egg-shell meal granularity 60 ~ 300 orders, egg-shell meal is by lactic acid and calcium carbonate chemistry reaction formula punishment in advance amount 5% ~ 75%, reaction times 30 ~ 180min, temperature of reaction is 30 ~ 55 ℃, lactic acid concn is 5wt% ~ 20wt%, after question response was finished, with the product suction filtration, reserved filtrate was for subsequent use;
(3) calcium lactate crystallization: the filtrate decompression of step (2) preparation is concentrated into volume percent 50% ~ 70%, places 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration, it is for subsequent use to get calcium lactate coarse crystallization body;
(4) the calcium lactate purifying is with dry: with the calcium lactate coarse crystallization body and function dehydrated alcohol wash-out of preparation in the step (3), wash-out solid-liquid volume ratio is 1:2 ~ 1:6, wash-out 40min, wash-out three times, suction filtration, 80 ℃ of dry calcium lactate products that get, product calcium lactate purity reaches 98%.
2. neutralizing under the eggshell vacuum environment as claimed in claim 1 prepares the method for calcium lactate, it is characterized in that be finely ground to 60 orders, 100 orders, 200 orders or 300 orders in the described step (1), it is for subsequent use to get egg-shell meal.
3. neutralizing under the eggshell vacuum environment as claimed in claim 1 prepares the method for calcium lactate, it is characterized in that 100-130 ℃ oven dry 25-30min in the described step (1), 80 ℃ of dry 2h.
4. neutralize under the eggshell vacuum environment as claimed in claim 1 and prepare the method for calcium lactate, it is characterized in that, vacuum tightness 0.04Mpa in the described step (2), egg-shell meal is by lactic acid and calcium carbonate chemistry reaction formula punishment in advance amount 15%, egg-shell meal granularity 100 orders, reaction times 45min, 40 ℃ of temperature of reaction, the solid-liquid mass ratio is 1:12.
5. neutralize under the eggshell vacuum environment as claimed in claim 1 and prepare the method for calcium lactate, it is characterized in that described step is concentrated into volume percent 50% with filtrate decompression in (3), place 5 ℃ of refrigerator and cooled to hide 4h the calcium lactate solution after concentrated, suction filtration gets calcium lactate coarse crystallization body.
6. neutralizing under the eggshell vacuum environment as claimed in claim 1 prepares the method for calcium lactate, it is characterized in that wash-out solid-liquid volume ratio is 1:4 in the described step (4).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316896A (en) * | 2013-06-27 | 2013-09-25 | 北京二商健力食品科技有限公司 | Processing method of eggshell powder |
| CN104230700A (en) * | 2014-09-29 | 2014-12-24 | 杨俊� | Production process for preparing calcium lactate through one-step synthesis method |
| CN109824504A (en) * | 2019-03-28 | 2019-05-31 | 阿坝师范学院 | The technique of Calcium Lactate from Egg Shells |
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| CN101172944A (en) * | 2006-11-01 | 2008-05-07 | 高新 | Method for producing calcium lactate with egg shell |
| CN102690191A (en) * | 2012-06-11 | 2012-09-26 | 广西工学院 | Method for producing calcium lactate by taking duck egg shell as raw material |
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2012
- 2012-10-24 CN CN2012104079282A patent/CN102887823A/en active Pending
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| CN101172944A (en) * | 2006-11-01 | 2008-05-07 | 高新 | Method for producing calcium lactate with egg shell |
| CN102690191A (en) * | 2012-06-11 | 2012-09-26 | 广西工学院 | Method for producing calcium lactate by taking duck egg shell as raw material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103316896A (en) * | 2013-06-27 | 2013-09-25 | 北京二商健力食品科技有限公司 | Processing method of eggshell powder |
| CN103316896B (en) * | 2013-06-27 | 2016-08-10 | 北京二商健力食品科技有限公司 | A kind of processing method of egg-shell meal |
| CN104230700A (en) * | 2014-09-29 | 2014-12-24 | 杨俊� | Production process for preparing calcium lactate through one-step synthesis method |
| CN109824504A (en) * | 2019-03-28 | 2019-05-31 | 阿坝师范学院 | The technique of Calcium Lactate from Egg Shells |
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Application publication date: 20130123 |