CN103539095A - Process for preparing food grade calcium hydrogen phosphate by ox bones - Google Patents
Process for preparing food grade calcium hydrogen phosphate by ox bones Download PDFInfo
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- CN103539095A CN103539095A CN201310557184.7A CN201310557184A CN103539095A CN 103539095 A CN103539095 A CN 103539095A CN 201310557184 A CN201310557184 A CN 201310557184A CN 103539095 A CN103539095 A CN 103539095A
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Abstract
The invention relates to a process for preparing food grade calcium hydrogen phosphate by ox bones. New raw materials for preparing food grade calcium hydrogen phosphate are adopted. The main process comprises the following steps: (1) processing calcium water of the ox bones, subjected to demineralization, through a coagulation and flocculation device; (2) filtering overflowed calcium water through a filtering groove; (3) aerating and micro-filtering the filtered calcium water; (4) preprocessing unslaked lime; (5) neutralizing; (6) filtering sediments generated during neutralizing, washing, carrying out spin-drying through a centrifugal machine, and carrying out pneumatic drying to obtain finished food grade calcium hydrogen phosphate. The process has the characteristics of low impurity content, low heavy metal and fluorine content, simple process, simplicity in raw material acquisition, simplicity and convenience in operation, stable product quality, low environmental pollution and the like.
Description
Technical field
The present invention is a kind of preparation technology of food-grade calcium hydrogen phosphate, belongs to biological chemistry, microorganism field, in particular with ox bone, prepares the technique of food-grade calcium hydrogen phosphate.
Background technology
The conventional food-grade calcium hydrogen phosphate method of preparing mainly contains thermal phosphoric acid method and wet phosphoric acid at present, and the power consumption of thermal phosphoric acid technique is large, cost is high, and production process produces a large amount of dust and toxic gas, and the product heavy metal content generating is high.The key of phosphoric acid by wet process is the purification of phosphoric acid by wet process, and its purifying method has two kinds: the one, and by adding defluorinating agent, removing heavy-metal and dearsenic agent that impurity is removed from phosphoric acid, the 2nd, by adding extraction agent to extract high-purity phosphoric acid from phosphoric acid by wet process.The purifying phosphoric acid that a kind of front method obtains is for food or prepare food-grade calcium hydrogen phosphate technology maturation not enough.The phosphoric acid purity that a kind of rear method obtains is slightly high, but extraction agent cost used is higher, and the raw material of these two kinds of methods is mainly phosphorus ore.Adopt phosphate ore processing legal system for food-grade calcium hydrogen phosphate have that phosphorus yield is low, environmental pollution serious, the shortcoming such as poor product quality (fluorine, arsenic, lead content are high).In order to reach the national standard of food-grade calcium hydrogen phosphate, need through complicated purification process, and increased production cost.
Some gelatin factories utilize the spent acid producing after skeletal grain pickling in gelatine production course at present, are the secondary calcium phosphate of raw material production feed grade.Although solved the spent acid in manufacturing of gelatin, process problem, calcium hydrophosphate fodder product price is low, and market demand is little, and economic benefit is remarkable not.
Summary of the invention
For the above-mentioned defect existing in prior art, it is low that the present invention aims to provide a kind of secondary calcium phosphate foreign matter content, and heavy metal, fluorine content is low, production cost is low, constant product quality, and the simple ox bone of operating procedure is prepared food-grade calcium hydrogen phosphate process technology scheme.
The present invention is achieved through the following technical solutions:
A technique of preparing food-grade calcium hydrogen phosphate with ox bone, 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) pre-treatment of unslaked lime;
(5) neutralizing treatment;
(6) throw out that neutralization generates filters, and after washing, whizzer dries, then obtains food-grade calcium hydrogen phosphate finished product through air stream drying.
Calcium water in described step (1) sucks mixing pit by intake pump, mix with the 10% coagulant solution-polyaluminium sulfate from liquid-storing box, the dosage of coagulating agent is 0.1L/L, again according to mixed solution: the ratio of 0.2% polyacrylamide=1:0.006, to add concentration be the non-ionic polyacrylamide of 0.2% food grade and mix 1min.Supernatant after flocculation enters filter vat by overflow.
Calcium clear overflow waterborne in described step (2) enters filter vat and further filters.The medium that filter vat adopts is activated alumina.
Aeration in described step (3)+micro-filtration process by the calcium water of processing through activated alumina under the suction function of suction pump through micro-filtrate membrane filtration.Calcium water promotes and enters membrane reactor through pump, and the aerating apparatus of opening subsequently reactor bottom carries out aeration, and 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 the settling on film surface to rinse suction stage, and whole flow process is controlled automatically by industrial computer.Calcium water adopts the mode of continuous water inlet, continuous aeration and water outlet at intermittence (suspending 2mi n after every water outlet 10mi n) in the operation scheme of this step, with decelerating membrane pollution.Microfiltration membrane aperture is the hollow-fibre membrane of 0.2 μ m, and material is polyvinylidene difluoride (PVDF) (PVDF), and the solid matter being trapped is attached to film silk outside surface, and periodically air-water flushing can be by its most of removal.
Unslaked lime pretreatment mode in described step (4) is: unslaked lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), slake is newborn through the separated large impurity of cyclone separator by ash after 72 hours, through 200 order reciprocating sieves, filter again, finally the ash breast after filtering is diluted to the stand-by ash breast that concentration is 3% (every 100mL is containing 3g lime).
Neutralizing treatment in described step (5) is after pretreated calcium water is got in synthesis tank with pump, then the ash breast that is 3% by concentration gets in synthesis tank with the flow velocity of 12L/min, and limit edged stirs, and stir speed (S.S.) is 80r/min.Temperature of reaction is 25 ℃.The pH value of liquid detect synthesis tank when adding ash charge breast in, when neutralizer pH value is 5.0, stops feeding in raw material, and continues to stir 1h, makes its final pH value be controlled at 5.8 ± 0.1.
The throw out generating in described step (6) is sent to whizzer through belt again after washing three times and dries, and the rotating speed of whizzer is 5000r/min.Work in-process after drying are sent to dehumidification system through belt again and carry out airflow drying, and the inlet temperature of air stream drying is 250-280 ℃, and temperature of outgoing air is below 80 ℃.
Method of the present invention is compared and is had the following advantages with traditional technology: adopted coagulation-microfiltration method to remove impurity, do not consumed phosphoric acid, reduced the exploitation of phosphate rock resource; Removal of impurities dosing used is few, and dust removal rate is high; Raw materials for production ox bone is not only produced secondary calcium phosphate, can also produce gelatin, and reduce costs.This product secondary calcium phosphate foreign matter content is low, the secondary calcium phosphate that heavy metal, fluorine content are produced far below phosphate ore processing method; This technique and traditional processing technology technology comparison both at home and abroad, have less investment, instant effect, and technical process is simple.Raw material is easy to get, easy and simple to handle, constant product quality, the feature such as environmental pollution is little.
Embodiment
Embodiment 1:
Detect pH value, the acid strength of calcium water, adjust pH value to 4.05, acid content is 0.27%.By 500L calcium water and concentration from liquid-storing box, be that 10% coagulant solution one bodied ferric sulfate pumps into mixing pit simultaneously and mixes, the dosage of coagulating agent is 51L, adding concentration is the non-ionic polyacrylamide of 0.2% food grade again, and dosage is 3.1L, mixes 1min.Supernatant after flocculation enters filter vat by overflow, and the activated alumina of take filters as filtration medium.
The calcium water of processing through activated alumina is entered continuously to microfiltration membrane reactor under the suction function of suction pump, the aerating apparatus of opening subsequently reactor bottom carries out continuous aeration, and aeration rate in service is 6L/h, regulates intake valve, control gas-water ratio is 5:1, and unnecessary gas is from bypass discharge leg.Entering film pressure is 1.5MPa, goes out film pressure 1.3MPa.
Unslaked lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), slake is newborn through the separated large impurity of cyclone separator by ash after 72 hours, through 200 order reciprocating sieves, filter, the ash breast that finally the ash breast after filtering is diluted to concentration and is 3% (every 100mL is containing 3g lime) is stand-by again.
Calcium water after processing is got in synthesis tank with pump, then the ash breast that is 3% by the concentration of handling well gets in synthesis tank with the flow velocity of 12L/min, limit edged stirs, and stir speed (S.S.) is 80r/min.Temperature of reaction is 25 ℃.The pH value of liquid detect synthesis tank when adding ash charge breast in, when neutralizer pH value is 5.0, stops feeding in raw material, and continues to stir 1h, and final pH value is 5.8.
The throw out generating is sent to whizzer and dries after microorganism qualified water is washed three times, and the rotating speed of whizzer is 5000r/mi n.Work in-process after drying are sent to dehumidification system through belt again and carry out airflow drying, and the inlet temperature of air stream drying is 280 ℃, and temperature of outgoing air is 79 ℃, and the product index obtaining is in Table one:
Table one
| Project | Index |
| The massfraction of secondary calcium phosphate (%) | 99.4 |
| The massfraction of loss on ignition (%) | 24.54 |
| The massfraction (%) of heavy metal (in Pb) | ≤0.001 |
| The massfraction of plumbous (Pb) | ≤0.0005 |
| The massfraction of arsenic (%) | ≤0.0002 |
| The massfraction of fluorochemical (%) | 0.0035 |
| The massfraction of hydrochloric acid insoluble substance (%) | 0.0327 |
Embodiment 2:
Detect pH value, the acid strength of calcium water, adjust pH value to 4.32, acid content is 0.28%.By 500L calcium water and concentration from liquid-storing box, be that 10% coagulant solution-bodied ferric sulfate pumps into mixing pit simultaneously and mixes, the dosage of coagulating agent is 50L, adding concentration is the non-ionic polyacrylamide of 0.2% food grade again, and dosage is 3.2L, mixes 1min.Supernatant after flocculation enters filter vat by overflow, and the activated alumina of take filters as filtration medium.
The calcium water of processing through activated alumina is entered continuously to microfiltration membrane reactor under the suction function of suction pump, the aerating apparatus of opening subsequently reactor bottom carries out continuous aeration, and aeration rate in service is 6L/h, regulates intake valve, control gas-water ratio is 5:1, and unnecessary gas is from bypass discharge leg.Entering film pressure is 1.5MPa, goes out film pressure 1.3MPa.
Unslaked lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), slake is newborn through the separated large impurity of cyclone separator by ash after 72 hours, through 200 order reciprocating sieves, filter, the ash breast that finally the ash breast after filtering is diluted to concentration and is 3% (every 100mL is containing 3g lime) is stand-by again.
Calcium water after processing is got in synthesis tank with pump, then the ash breast that is 3% by the concentration of handling well gets in synthesis tank with the flow velocity of 12L/min, limit edged stirs, and stir speed (S.S.) is 80r/min.Temperature of reaction is 25 ℃.The pH value of liquid detect synthesis tank when adding ash charge breast in, when neutralizer pH value is 5.0, stops feeding in raw material, and continues to stir 1h, and final pH value is 5.7.
The throw out generating is sent to whizzer and dries after microorganism qualified water is washed three times, and the rotating speed of whizzer is 5000r/mi n.Work in-process after drying are sent to dehumidification system through belt again and carry out airflow drying, and the inlet temperature of air stream drying is 280 ℃, and temperature of outgoing air is 79 ℃, and the product index obtaining is table two again:
Table two
| Project | Index |
| The massfraction of secondary calcium phosphate (%) | 99.6 |
| The massfraction of loss on ignition (%) | 24.86 |
| The massfraction (%) of heavy metal (in Pb) | ≤0.001 |
| The massfraction of plumbous (Pb) | ≤0.0005 |
| The massfraction of arsenic (%) | ≤0.0002 |
| The massfraction of fluorochemical (%) | 0.0028 |
| The massfraction of hydrochloric acid insoluble substance (%) | 0.0365 |
Embodiment 3:
Detect pH value, the acid strength of calcium water, adjust pH value to 4.15, acid content is 0.3%.By 500L calcium water and concentration from liquid-storing box, be that 10% coagulant solution-bodied ferric sulfate pumps into mixing pit simultaneously and mixes, the dosage of coagulating agent is 52L, adding concentration is the non-ionic polyacrylamide of 0.2% food grade again, and dosage is 3.2L, mixes 1min.Supernatant after flocculation enters filter vat by overflow, and the activated alumina of take filters as filtration medium.
The calcium water of processing through activated alumina is entered continuously to microfiltration membrane reactor under the suction function of suction pump, the aerating apparatus of opening subsequently reactor bottom carries out continuous aeration, and aeration rate in service is 6L/h, regulates intake valve, control gas-water ratio is 5:1, and unnecessary gas is from bypass discharge leg.Entering film pressure is 1.5MPa, goes out film pressure 1.3MPa.
Unslaked lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), slake is newborn through the separated large impurity of cyclone separator by ash after 72 hours, through 200 order reciprocating sieves, filter, the ash breast that finally the ash breast after filtering is diluted to concentration and is 3% (every 100mL is containing 3g lime) is stand-by again.
Calcium water after processing is got in synthesis tank with pump, then the ash breast that is 3% by the concentration of handling well gets in synthesis tank with the flow velocity of 12L/min, limit edged stirs, and stir speed (S.S.) is 80r/min.Temperature of reaction is 25 ℃.The pH value of liquid detect synthesis tank when adding ash charge breast in, when neutralizer pH value is 5.0, stops feeding in raw material, and continues to stir 1h, and final pH value is 5.8.
The throw out generating is sent to whizzer and dries after microorganism qualified water is washed three times, and the rotating speed of whizzer is 5000r/mi n.Work in-process after drying are sent to dehumidification system through belt again and carry out airflow drying, and the inlet temperature of air stream drying is 280 ℃, and temperature of outgoing air is 79 ℃, and the product index obtaining is table three again:
Table three
| Project | Index |
| The massfraction of secondary calcium phosphate (%) | 99.5 |
| The massfraction of loss on ignition (%) | 25.34 |
| The massfraction (%) of heavy metal (in Pb) | ≤0.001 |
| The massfraction of plumbous (Pb) | ≤0.0005 |
| The massfraction of arsenic (%) | ≤0.0002 |
| The massfraction of fluorochemical (%) | 0.0025 |
| The massfraction of hydrochloric acid insoluble substance (%) | 0.0325 |
Claims (7)
1. with ox bone, prepare a technique for food-grade calcium hydrogen phosphate, it is characterized in that mainly comprising the following 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) pre-treatment of unslaked lime;
(5) neutralizing treatment;
(6) throw out that neutralization generates filters, and after washing, whizzer dries, then obtains food-grade calcium hydrogen phosphate finished product through air stream drying.
2. a kind of technique of preparing food-grade calcium hydrogen phosphate with ox bone according to claim 1, it is characterized in that: the calcium water in described step (1) sucks mixing pit by intake pump, mix with coagulant solution-bodied ferric sulfate of 10% from liquid-storing box, the dosage of coagulating agent is 0.1L/L, again according to mixed solution: the ratio of 0.2% polyacrylamide=1:0.006, to add concentration be the non-ionic polyacrylamide of 0.2% food grade and mix 1min, and the supernatant after flocculation enters filter vat by overflow.
3. a kind of technique of preparing food-grade calcium hydrogen phosphate with ox bone according to claim 1, is characterized in that: the calcium clear overflow waterborne in described step (2) enters filter vat and filters, and the medium that filter vat adopts is activated alumina.
4. a kind of technique of preparing food-grade calcium hydrogen phosphate with ox bone according to claim 1, it is characterized in that: the aeration in described step (3)+micro-filtration process by the calcium water of processing through activated alumina under the suction function of suction pump through micro-filtrate membrane filtration, calcium water promotes and enters membrane reactor through pump, in service is 6L/h by aeration control, regulate intake valve, control gas-water ratio is 5:1, continuous aeration and intermittently water outlet microfiltration membrane aperture are the hollow-fibre membrane of 0.2 μ m, and material is polyvinylidene difluoride (PVDF) (PVDF).
5. a kind of technique of preparing food-grade calcium hydrogen phosphate with ox bone according to claim 1, it is characterized in that: the unslaked lime pretreatment mode in described step (4) is: unslaked lime and water are carried out to slake in 1:4 ratio (1 kilogram of raw lime adds 4 premium on currency), slake is newborn through the separated large impurity of cyclone separator by ash after 72 hours, through 200 order reciprocating sieves, filter, the ash breast that finally the ash breast after filtering is diluted to concentration and is 3% (every 100mL is containing 3g lime) is stand-by again.
6. a kind of technique of preparing food-grade calcium hydrogen phosphate with ox bone according to claim 1, it is characterized in that: the neutralizing treatment in described step (5) is after pretreated calcium water is got in synthesis tank with pump, the ash breast that is 3% by concentration is again got in synthesis tank with the flow velocity of 12L/min, stir speed (S.S.) is 80r/min, temperature of reaction is 25 ℃, the pH value of liquid detect synthesis tank when adding ash charge breast in, when neutralizer pH value is 5.0, continue to stir 1h, make its final pH value be controlled at 5.8 ± 0.1.
7. a kind of technique of preparing food-grade calcium hydrogen phosphate with ox bone according to claim 1, it is characterized in that: the throw out generating in step (6) is sent to whizzer through belt again after washing three times and dries, the rotating speed of whizzer is 5000r/min, work in-process after drying are sent to dehumidification system through belt again and carry out airflow drying, the inlet temperature of air stream drying is 250-280 ℃, and temperature of outgoing air is below 80 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621379A (en) * | 2016-04-13 | 2016-06-01 | 四川绵竹市盘龙矿物质有限责任公司 | Improved three-stage neutralization crystallization method in feed-grade calcium hydrogen phosphate production technique |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004244291A (en) * | 2003-02-17 | 2004-09-02 | Ngk Spark Plug Co Ltd | Calcium hydrogen phosphate powder, powder for calcium phosphate based paste, calcium phosphate based paste kneader unit and method of manufacturing calcium hydrogen phosphate powder |
| CN102502554A (en) * | 2011-11-03 | 2012-06-20 | 蚌埠丰原明胶有限公司 | Method for preparing calcium hydrophosphate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004244291A (en) * | 2003-02-17 | 2004-09-02 | Ngk Spark Plug Co Ltd | Calcium hydrogen phosphate powder, powder for calcium phosphate based paste, calcium phosphate based paste kneader unit and method of manufacturing calcium hydrogen phosphate powder |
| CN102502554A (en) * | 2011-11-03 | 2012-06-20 | 蚌埠丰原明胶有限公司 | Method for preparing calcium hydrophosphate |
Non-Patent Citations (2)
| Title |
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| 李登好等: "盐酸浸取兽骨制备食品级磷酸氢钙", 《辽宁化工》, vol. 28, no. 1, 31 January 1999 (1999-01-31), pages 47 - 48 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621379A (en) * | 2016-04-13 | 2016-06-01 | 四川绵竹市盘龙矿物质有限责任公司 | Improved three-stage neutralization crystallization method in feed-grade calcium hydrogen phosphate production technique |
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