CN103539094B - A kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone - Google Patents
A kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone Download PDFInfo
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Abstract
The present invention relates to a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone, is to utilize the raw material-ox bone of gelatine production course to prepare toothpaste grade calcium hydrophosphate, mainly comprises the following steps: (1) is by the calcium water process coagulation-flocculation device after ox bone demineralization; (2) the calcium water overflowing is filtered through filter pocket; (3) the calcium water filtering carries out the step of aeration+micro-filtration; (4) pretreatment of quick lime; (5) step of neutralisation treatment; (6) neutralization generates calcium monohydrogen phosphate sediment, leaves standstill, and absorption upper strata calcium water, stirs and add stabilizer treatment; (7) filter through the sediment of stabilizer treatment, after washing, centrifuge dries, then obtains toothpaste grade calcium hydrophosphate finished product through airflow drying. This product reduces the shortcomings such as fluorine, arsenic, lead content height, and production process environmental pollution is little, and integrated cost is low.
Description
Technical field
The present invention relates to a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone, belong to biochemistry, microorganism field,Especially prepare the technique of toothpaste grade calcium hydrophosphate with ox bone.
Background technology
Toothpaste grade calcium hydrophosphate is the high-quality rubbing agent of generally acknowledging in the world, compared with ordinary toothpaste rubbing agent-calcium carbonate, and toolHave friction valve moderate, etch factor is little, does not damage enamel, good with compatibility of drugs, and other compositions are had to good adsorptivityEtc. advantage. At present developed country has banned use of calcium carbonate as toothpaste abrasives, therefore on international market to toothpaste level phosphoric acidThe demand of hydrogen calcium increases increasingly, and the main manufacturer of existing domestic toothpaste is also all developing taking toothpaste grade calcium hydrophosphate as frictionThe high-grade toothpaste of agent is as developing direction, and toothpaste grade calcium hydrophosphate has good development prospect.
The method of at present synthetic toothpaste grade calcium hydrophosphate mainly contains: sodium hydrogen phosphate-calcium dihydrogen phosphate method, sodium hydrogen phosphateMethod, thermal phosphoric acid method, wet phosphoric acid purifying method. This several method respectively has pluses and minuses, sodium hydrogen phosphate-calcium dihydrogen phosphate method: nothingThree waste discharge, but reaction condition control requirement is high; Sodium hydrogen phosphate method: derive from the sodium hydrogen phosphate of phosphoric acid by wet process containing higherSulfate and the existence of other impurity, particularly sulfate can make reaction generate calcium sulfate to enter in toothpaste lotion is hardened,Therefore must purify by recrystallization, the recrystallization of sodium hydrogen phosphate, labour intensity is excessive, and process is loaded down with trivial details, and phosphorus loss is high. SeparatelyOutward, when synthetic calcium monohydrogen phosphate, unstable if the improper crystallization water that easily causes is controlled in reaction, carbonate is excessive, and pH value and stability are notThe quality problems such as qualified. Thermal phosphoric acid method can produce a large amount of sodium chloride and carbon dioxide while producing calcium monohydrogen phosphate, waste resource,Contaminated environment; The key of wet phosphoric acid purifying method is the purification of phosphoric acid by wet process. Its purification method has two kinds: the one, and de-by addingFluorine agent, removing heavy-metal and Hydrodearsenic Catalyst are removed impurity from phosphoric acid, and the 2nd, by adding extractant to extract from phosphoric acid by wet processHigh-purity phosphoric acid. The purifying phosphoric acid that a kind of front method obtains is for food or prepare food-grade calcium hydrogen phosphate technology and become not enoughRipe. The phosphoric acid purity that a kind of rear method obtains is slightly high, but extractant cost used is higher.
At present some gelatin factories utilize the spent acid that produces after skeletal grain pickling in gelatine production course to produce feed for raw materialThe calcium monohydrogen phosphate of level. Process problem although solved the spent acid in manufacturing of gelatin, product price is low, and market demand is little.
Summary of the invention
For the above-mentioned defect existing in prior art, the present invention aims to provide a kind of simple to operate, and production cost is lower,Improve phosphorus yield, reduce fluorine, arsenic, lead content high, prepare the technical scheme of toothpaste grade calcium hydrophosphate with ox bone.
The present invention adopts the raw material-ox bone of gelatine production course to prepare the technique of toothpaste grade calcium hydrophosphate, be by belowTechnical scheme realizes:
It mainly comprises following concrete steps:
(1) by the calcium water process coagulation-flocculation device after ox bone demineralization;
(2) the calcium water overflowing is filtered through filter pocket;
(3) the calcium water filtering carries out aeration+micro-filtration;
(4) pretreatment of quick lime;
(5) neutralisation treatment;
(6) neutralization generates calcium monohydrogen phosphate sediment, leaves standstill, and absorption upper strata calcium water, stirs and add stabilizing agent;
(7) filter through the sediment of stabilizer treatment, after washing, centrifuge dries, then obtains toothpaste level phosphorus through airflow dryingAcid hydrogen calcium finished product.
Calcium water in described step (1) sucks mixing pit by intake pump, with 10% coagulant solution from liquid reserve tank-poly-Close aluminum sulfate and mix, the dosage of coagulant is 0.1L/L, then according to the ratio of mixed liquor: 0.2% polyacrylamide=1:0.006Example, to add concentration be the non-ionic polyacrylamide of 0.2% food stage and mix 1min. Supernatant after flocculation is by overflowEnter lautertuns.
Calcium clear overflow waterborne in described step (2) enters lautertuns and filters, and the medium that lautertuns adopts is activeAluminium oxide.
Aeration+micro-filtration in described step (3) is processed the suction in suction pump by the calcium water through activated alumina processingUnder effect, through micro-filtrate membrane filtration, calcium water promotes and enters membrane reactor through pump, and the aerator of opening subsequently reactor bottom carries outAeration, in service is 6L/h by aeration control, regulates intake valve, and control gas-water ratio is 5:1, and unnecessary gas is from bypass discharge leg.Aerating system does not move during film suction, and during film stop pumping, starts to start, and is accumulated in film surface to rinse suction stageDeposit, whole flow process is controlled automatically by industrial computer. Calcium water adopts water inlet, continuous aeration continuously in the method for operation of this stepWith the mode of water outlet at intermittence (suspending 2min after every water outlet 10min), with decelerating membrane pollution. Micro-filtration membrane aperture is the hollow of 0.2 μ mTunica fibrosa, material is Kynoar (PVDF), the solid matter being trapped is attached to film silk outer surface, periodically air water punchingWashing can be by its most of removal.
Quick lime pretreatment mode in described step (4) is: by quick lime and water, in 1:4 ratio, (1 kilogram of raw lime adds4 premium on currency) carry out slake, slake separated large impurity by ash breast through cyclone separator after 72 hours, then filtered through 200 order reciprocating sieves,Finally the ash breast after filtering is diluted to the stand-by ash breast that concentration is 3% (every 100mL is containing 3g lime).
Neutralisation treatment in described step (5) is after pretreated calcium water pump is got in synthesis tank, then by concentrationBe that 3% ash breast is got in synthesis tank with the flow velocity of 12L/min, limit edged stirs, and stir speed (S.S.) is 80r/min. ReactionTemperature is 25 DEG C. The pH value of liquid detect synthesis tank in adding ash charge breast in, in the time that neutralizer pH value is 5.0, stops addingMaterial, continues to stir 1h, makes its final pH value be controlled at 5.8 ± 0.1.
In described step (6), stabilizing agent adopts magnesium hydroxide, and addition is 0.55% of calcium monohydrogen phosphate weight.
The sediment generating in described step (7) is sent to centrifuge through belt again after washing three times and dries, centrifugeRotating speed is 5000r/min. Semi-finished product after drying are sent to drying system through belt again and carry out airflow drying, the entering of pneumatic conveying dryingAir temperature is 250-280 DEG C, and temperature of outgoing air is below 80 DEG C.
Method of the present invention has the following advantages compared with traditional handicraft: do not consume phosphoric acid, reduced opening of phosphate rock resourceAdopt; Removal of impurities dosing used is few, and expense is extremely low, and dust removal rate is high; The raw material ox bone of production and application not only can be producedCalcium monohydrogen phosphate, can also be used to produce gelatin, and production cost is reduced, and economic benefit is greater than traditional handicraft, and raw material sources are extensive,The calcium monohydrogen phosphate impurity content of producing is low, the calcium monohydrogen phosphate that heavy metal, fluorine content are produced far below phosphate ore processing method; This techniqueWith the comparison of domestic and international traditional processing technology technology, there is small investment, instant effect, technological process is short, and advanced technology is reasonable, and raw material is easy, easy and simple to handle, without byproduct production, constant product quality, the feature such as environmental pollution is little.
Detailed description of the invention
Embodiment 1:
Detect pH value, the acid strength of calcium water, adjust pH value to 4.05, acid content is 0.3%. By 500L calcium water with fromThe concentration of liquid reserve tank is that 10% coagulant solution-bodied ferric sulfate pumps into mixing pit simultaneously and mixes, the dosage of coagulantFor 50L, then to add concentration be the non-ionic polyacrylamide of 0.2% food stage, and dosage is 3L, mixes 1min. After flocculationSupernatant enter lautertuns by overflow, filter taking activated alumina as filter medium.
To under the swabbing action of suction pump, enter continuously micro-filtration membrane reactor through the calcium water of activated alumina processing, withThe aerator of rear unlatching reactor bottom carries out continuous aeration, and aeration rate in service is 6L/h, regulates intake valve, controls air waterThan being 5:1, unnecessary gas is from bypass discharge leg. Entering film pressure is 1.5MPa, goes out film pressure 1.3MPa.
Quick lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), and slake is newborn by ash after 72 hoursSeparate large impurity through cyclone separator, then filter through 200 order reciprocating sieves, finally the ash breast after filtering being diluted to concentration is 3%The ash breast of (every 100mL is containing 3g lime) is stand-by.
Calcium water after treatment is got in synthesis tank with pump, then the ash breast that is 3% by the concentration of handling well is with 12L/min'sFlow velocity is got in synthesis tank, and limit edged stirs, and stir speed (S.S.) is 80r/min. Reaction temperature is 25 DEG C. Adding ash charge breastDetect the pH value of liquid in synthesis tank simultaneously, in the time that neutralizer pH value is 5.0, stop feeding in raw material, continue to stir 1h, final pH value is5.8. Neutralization generates calcium monohydrogen phosphate sediment, leaves standstill 0.5h, absorbs upper strata calcium water, stirs and adds 260g stabilizing agent magnesium hydroxide;The product generating is sent to centrifuge and dries after microorganism qualified water is washed three times, and the rotating speed of centrifuge is 5000r/min. Get rid ofSemi-finished product after dry are sent to drying system through belt again and carry out airflow drying, and the EAT of pneumatic conveying drying is 280 DEG C, air draftTemperature is 79 DEG C, and the product index obtaining is in table one:
Table one
| Project | Index |
| Calcium oxide (w/%) | 32.1 |
| Phosphorus pentoxide (w/%) | 41.8 |
| Whiteness (degree) | 98 |
| PH (20% suspension) | 7.5 |
| Fineness (< 45 μ m, w/%) | 99.8 |
| 20g product water absorption/ml | 5.8 |
| Apparent density (g/cm3) | 0.9 |
| Stability | By test |
| Fluoride stability test | By test |
| Burning decrement (w/%) | 25.54 |
| 60 DEG C of dry vectors (w/%) | 0.545 |
| Heavy metal (in Pb, w/%)≤ | 0.002 |
| Arsenic (w/%)≤ | 0.0003 |
| Iron (w/%) | 0.0065 |
| Fluorine (w/%) | 0.0025 |
| Chloride (w/%)≤ | 0.03 |
| Carbonate | By test |
| Sulfate (w/%)≤ | 0.5 |
| Sulfide | By test |
| Hydrochloric acid insoluble substance (w/%) | 0.132 |
| Total plate count (individual/g) | 80 |
| Excrement colibacillus group | Do not detect 3 --> |
| Pseudomonas aeruginosa | Do not detect |
| Staphylococcus aureus | Do not detect |
| Mould and saccharomycete sum (individual/g) | 50 |
Embodiment 2:
Detect pH value, the acid strength of calcium water, adjust pH value to 4.35, acid content is 0.28%. By 500L calcium water and nextBe that 10% coagulant solution-bodied ferric sulfate pumps into mixing pit simultaneously and mixes from the concentration of liquid reserve tank, the adding of coagulantAmount is for 52L, then to add concentration be the non-ionic polyacrylamide of 0.2% food stage, and dosage is 3.5L, mixes 1min. WaddingSupernatant after solidifying enters lautertuns by overflow, filters taking activated alumina as filter medium.
To under the swabbing action of suction pump, enter continuously micro-filtration membrane reactor through the calcium water of activated alumina processing, withThe aerator of rear unlatching reactor bottom carries out continuous aeration, and aeration rate in service is 6L/h, regulates intake valve, controls air waterThan being 5:1, unnecessary gas is from bypass discharge leg. Entering film pressure is 1.5MPa, goes out film pressure 1.3MPa.
Quick lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), and slake is newborn by ash after 72 hoursSeparate large impurity through cyclone separator, then filter through 200 order reciprocating sieves, finally the ash breast after filtering being diluted to concentration is 3%The ash breast of (every 100mL is containing 3g lime) is stand-by.
Calcium water after treatment is got in synthesis tank with pump, then the ash breast that is 3% by the concentration of handling well is with 12L/min'sFlow velocity is got in synthesis tank, and limit edged stirs, and stir speed (S.S.) is 80r/min. Reaction temperature is 25 DEG C. Adding ash charge breastDetect the pH value of liquid in synthesis tank simultaneously, in the time that neutralizer pH value is 5.0, stop feeding in raw material, continue to stir 1h, final pH value is5.8. Neutralization generates calcium monohydrogen phosphate sediment, leaves standstill 0.5h, absorbs upper strata calcium water, stirs and adds 260g stabilizing agent magnesium hydroxide;The product generating is sent to centrifuge and dries after microorganism qualified water is washed three times, and the rotating speed of centrifuge is 5000r/min. Get rid ofSemi-finished product after dry are sent to drying system through belt again and carry out airflow drying, and the EAT of pneumatic conveying drying is 280 DEG C, air draftTemperature is 79 DEG C, and the product index obtaining is in table two:
Table two
| Project | Index |
| Calcium oxide (w/%) | 31.9 |
| Phosphorus pentoxide (w/%) | 41.6 |
| Whiteness (degree) | 98 |
| PH (20% suspension) | 7.4 |
| Fineness (< 45 μ m, w/%) | 99.8 |
| 20g product water absorption/ml | 5.9 |
| Apparent density (g/cm3) | 0.96 |
| Stability | By test |
| Fluoride stability test | By test |
| Burning decrement (w/%) | 25.36 |
| 60 DEG C of dry vectors (w/%) | 0.53 |
| Heavy metal (in Pb, w/%)≤ | 0.002 |
| Arsenic (w/%)≤ | 0.0003 |
| Iron (w/%) | 0.0056 4 --> |
| Fluorine (w/%) | 0.0015 |
| Chloride (w/%)≤ | 0.03 |
| Carbonate | By test |
| Sulfate (w/%)≤ | 0.5 |
| Sulfide | By test |
| Hydrochloric acid insoluble substance (w/%) | 0.145 |
| Total plate count (individual/g) | 40 |
| Excrement colibacillus group | Do not detect |
| Pseudomonas aeruginosa | Do not detect |
| Staphylococcus aureus | Do not detect |
| Mould and saccharomycete sum (individual/g) | 20 |
Buy and execute example 3:
Detect pH value, the acid strength of calcium water, adjust pH value to 4.0, acid content is 0.31%. By 500L calcium water with fromThe concentration of liquid reserve tank is that 10% coagulant solution-bodied ferric sulfate pumps into mixing pit simultaneously and mixes, the dosage of coagulantFor 50L, then to add concentration be the non-ionic polyacrylamide of 0.2% food stage, and dosage is 3.5L, mixes 1min. FlocculationAfter supernatant enter lautertuns by overflow, filter taking activated alumina as filter medium.
To under the swabbing action of suction pump, enter continuously micro-filtration membrane reactor through the calcium water of activated alumina processing, withThe aerator of rear unlatching reactor bottom carries out continuous aeration, and aeration rate in service is 6L/h, regulates intake valve, controls air waterThan being 5:1, unnecessary gas is from bypass discharge leg. Entering film pressure is 1.5MPa, goes out film pressure 1.3MPa.
Quick lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), and slake is newborn by ash after 72 hoursSeparate large impurity through cyclone separator, then filter through 200 order reciprocating sieves, finally the ash breast after filtering being diluted to concentration is 3%The ash breast of (every 100mL is containing 3g lime) is stand-by.
Calcium water after treatment is got in synthesis tank with pump, then the ash breast that is 3% by the concentration of handling well is with 12L/min'sFlow velocity is got in synthesis tank, and limit edged stirs, and stir speed (S.S.) is 80r/min. Reaction temperature is 25 DEG C. Adding ash charge breastDetect the pH value of liquid in synthesis tank simultaneously, in the time that neutralizer pH value is 5.0, stop feeding in raw material, continue to stir 1h, final pH value is5.8. Neutralization generates calcium monohydrogen phosphate sediment, leaves standstill 0.5h, absorbs upper strata calcium water, stirs and adds 260g stabilizing agent magnesium hydroxide;The product generating is sent to centrifuge and dries after microorganism qualified water is washed three times, and the rotating speed of centrifuge is 5000r/min. Get rid ofSemi-finished product after dry are sent to drying system through belt again and carry out airflow drying, and the EAT of pneumatic conveying drying is 280 DEG C, air draftTemperature is 79 DEG C, and the product index obtaining is in table three:
Table three
| Project | Index |
| Calcium oxide (w/%) | 31.6 |
| Phosphorus pentoxide (w/%) | 42.0 |
| Whiteness (degree) | 97 |
| PH (20% suspension) | 7.6 |
| Fineness (< 45 μ m, w/%) | 99.5 |
| 20g product water absorption/ml | 5.6 |
| Apparent density (g/cm3) | 0.94 5 --> |
| Stability | By test |
| Fluoride stability test | By test |
| Burning decrement (w/%) | 26.02 |
| 60 DEG C of dry vectors (w/%) | 0.52 |
| Heavy metal (in Pb, w/%)≤ | 0.002 |
| Arsenic (w/%)≤ | 0.0003 |
| Iron (w/%) | 0.0045 |
| Fluorine (w/%) | 0.0023 |
| Chloride (w/%)≤ | 0.03 |
| Carbonate | By test |
| Sulfate (w/%)≤ | 0.5 |
| Sulfide | By test |
| Hydrochloric acid insoluble substance (w/%) | 0.168 |
| Total plate count (individual/g) | 50 |
| Excrement colibacillus group | Do not detect |
| Pseudomonas aeruginosa | Do not detect |
| Staphylococcus aureus | Do not detect |
| Mould and saccharomycete sum (individual/g) | 10 |
Claims (6)
1. a technique of preparing toothpaste grade calcium hydrophosphate with ox bone, is characterized in that mainly comprising the following steps:
(1) by calcium water after ox bone demineralization through coagulation-flocculation device: calcium water sucks mixing pit by intake pump, and from liquid reserve tank10% coagulant solution-polymeric ferrous sulphate solution mix, the dosage of coagulant solution is 0.1L/L, then according to mixingThe ratio of liquid: 0.2% polyacrylamide=1:0.006, add concentration be 0.2% food stage non-ionic polyacrylamide alsoMix 1min, the supernatant after flocculation enters lautertuns by overflow;
(2) the calcium water overflowing is filtered through filter pocket;
(3) the calcium water filtering carries out the step of aeration+micro-filtration: the calcium water after filtration enters aperture under the swabbing action of suction pumpBe micro-filtration membrane reactor 0.2 μ m, that material is Kynoar, open the aerator of reactor bottom, by aeration rate controlBe made as 6L/h, gas-water ratio control is 5:1, and unnecessary gas is from bypass discharge leg, and the method for operation of calcium water adopts water inlet continuously, exposes to the sun continuouslyAfter gas and intermittently water outlet-every water outlet 10min, suspend the mode of 2min, with decelerating membrane pollution;
(4) pretreatment of quick lime;
(5) neutralisation treatment step;
(6) neutralization generates calcium monohydrogen phosphate sediment, leaves standstill, and absorption upper strata calcium water, stirs and add the stable step of processing of stabilizing agent;
(7) filter through the sediment of stabilizer treatment, after washing, centrifuge dries, then obtains toothpaste level phosphoric acid hydrogen through airflow dryingCalcium finished product.
2. a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone according to claim 1, is characterized in that: described stepSuddenly the clear overflow waterborne of the calcium in (2) enters lautertuns and further filters, and the medium that lautertuns adopts is activated alumina.
3. a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone according to claim 1, is characterized in that described stepSuddenly the quick lime pretreatment mode in (4) is: quick lime and water are added to 4 premium on currency in 1:4 ratio-1 kilogram of raw lime and disappearWith, slake separated large impurity by ash breast through cyclone separator after 72 hours, then filtered through 200 order reciprocating sieves, after finally filteringAsh breast add the ash breast that dilution proportion to the concentration of 3g lime is 3% by every 100mL stand-by.
4. a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone according to claim 1, is characterized in that: described stepSuddenly the neutralisation treatment in (5) is after pretreated calcium water pump is got in synthesis tank, then the ash breast that is 3% by concentration withThe flow velocity of 12L/min is got in synthesis tank, and reaction temperature control is 25 DEG C, and stir speed (S.S.) control is 80r/min, and limit edged entersRow stirs, and monitors the pH value of liquid in synthesis tank simultaneously, in the time that pH value is 5.0, stops feeding in raw material, and continues to stir 1h, makes it finalPH value is controlled at 5.8 ± 0.1.
5. a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone according to claim 1, is characterised in that: described step(6) in, stabilizing agent adopts magnesium hydroxide, and addition is 0.55% of calcium monohydrogen phosphate weight.
6. a kind of technique of preparing toothpaste grade calcium hydrophosphate with ox bone according to claim 1, is characterized in that: step(7) sediment generating in is sent to centrifuge through belt again after washing three times and dries, and the rotating speed of centrifuge is 5000r/min,Semi-finished product after drying are sent to drying system through belt again and carry out airflow drying, and the EAT of pneumatic conveying drying is 250-280DEG C, temperature of outgoing air is below 80 DEG C.
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| CN101549862A (en) * | 2009-05-18 | 2009-10-07 | 中国—阿拉伯化肥有限公司 | A method for wet phosphoric acid producing high pure calcium hydrogen orthophosphate |
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| CN101549862A (en) * | 2009-05-18 | 2009-10-07 | 中国—阿拉伯化肥有限公司 | A method for wet phosphoric acid producing high pure calcium hydrogen orthophosphate |
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| 畜骨生产磷酸氢钙工艺方法;赵景联;《河南科技》;19921231;第25页，第27页 * |
| 盐酸浸取兽骨制备食品级磷酸氢钙;李登好等;《辽宁化工》;19990131;第28卷(第1期);第47-48页 * |
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