CN104276562A - Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon - Google Patents
Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon Download PDFInfo
- Publication number
- CN104276562A CN104276562A CN201410595601.1A CN201410595601A CN104276562A CN 104276562 A CN104276562 A CN 104276562A CN 201410595601 A CN201410595601 A CN 201410595601A CN 104276562 A CN104276562 A CN 104276562A
- Authority
- CN
- China
- Prior art keywords
- washes
- activated carbon
- phosphoric acid
- washing wastewater
- hydrogen phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Fodder In General (AREA)
- Processing Of Solid Wastes (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon. A preparation process is mainly divided into four process steps: (1) pretreatment; (2) reactive synthesis; (3) filtration; and (4) product drying. The preparation process specifically comprises the following steps: by adopting the washing wastewater produced in a production process of phosphoric acid process wooden activated carbon as a raw material, firstly performing pretreatment on the washing wastewater by adopting a sedimentation auxiliary agent namely a polyacrylamide solution, and removing a great number of micro black activated carbon powder particles commonly contained in the washing wastewater after the raw material is pretreated; and adding a certain quantity of calcium hydroxide solutions to perform reactive synthesis, and performing further neutralization reaction to prepare a feed-grade calcium hydrogen phosphate product. By adopting the method for preparing feed-grade calcium hydrogen phosphate disclosed by the invention, the difficult problem that a great number of washing wastewater generated by wooden activated carbon manufacturers is hard to treat can be solved; and the method for preparing feed-grade calcium hydrogen phosphate can be used for creating economic values and solving the environmental pollution, and is of an environment-friendly production process with good economic benefits and little environment pollution.
Description
technical field:
The invention belongs to phosphorous chemical industry field, be specifically related to a kind of method utilizing the washes in phosphoric acid method wood activated charcoal production process to prepare calcium hydrophosphate fodder.
technical background:
Traditional technology is prepared wood activated charcoal and is mainly contained Physical, chemical method two kinds of preparation technologies, and Physical adopts water vapour to prepare gac as activator, and the higher production cost that causes of energy consumption is high; Chemical method adopts liquor zinci chloridi as activator, exists and pollutes the difficult problems such as large, environmental protection pressure is large.Phosphoric acid is generally adopted to prepare wood activated charcoal as activator at present both at home and abroad, the a large amount of phosphorous washes produced in its production process is difficult to process, most manufacturer all adopts limestone vegetation rear outer row's process up to standard, and this treatment process adds production cost virtually.
The washes composition of phosphoric acid method wood activated charcoal is mainly phosphorous 1% ~ 4%(in Vanadium Pentoxide in FLAKES) the aqueous solution, other foreign matter contents are lower, especially F and heavy metal, wherein Oil repellent is 0.0005% ~ 0.001%, heavy metal content is less than 0.0001%(in As), the phosphor resource can recycled contained by it prepares the higher calcium hydrophosphate fodder product of added value, turn waste into wealth and add economic benefit, mother liquor after recovery can use as gac wash water again, reduce water of productive use cost and cost of sewage disposal, achieve production waste zero release, solve environmental pollution problem, really realize Enterprise Circular Economy.
summary of the invention:
Object of the present invention recycles the washes of phosphoric acid method wood activated charcoal, be mainly phosphorous 1% ~ 4%(in its composition in Vanadium Pentoxide in FLAKES) the aqueous solution, other foreign matter contents are lower, and the phosphor resource recycled contained by it prepares the higher calcium hydrophosphate fodder product of added value.
A kind of washes utilizing activated carbon of phosphoric acid method to produce of the present invention prepares the method for calcium hydrophosphate fodder, and this preparation technology is mainly divided into four processing steps: 1. pre-treatment; 2. Reactive Synthesis; 3. filter; 4. product drying.Be specially: with the washes produced in phosphoric acid method wood activated charcoal production process for raw material, 1. pre-treatment, first the settling aids polyacrylamide solution adopted carries out pre-treatment to washes, and raw material removes the black activity charcoal powder particle trickle in a large number often contained in washes after pretreatment; 2. Reactive Synthesis, adds a certain amount of aqua calcis and carries out Reactive Synthesis, by a step neutralization reaction, prepares calcium hydrophosphate fodder product; Concrete technology parameter is: get a certain amount of washes, add the polyacrylamide solution that a certain amount of mass concentration is 0.1% wherein, make the content of polyacrylamide in solution in mass concentration 0.01% ~ 0.05%, filter after leaving standstill 6h, the aqua calcis of a certain amount of solid content 60% ~ 70% is added in filtrate, control temperature of reaction 40 DEG C ~ 60 DEG C, reaction times 1 h ~ 3h; Stirring velocity 150rpm ~ 400rpm, pH value 4 ~ 6, until reaction terminates; 3. filter, adopt vacuum filtration mode to filter; 4. product drying, filter cake is placed on 90 DEG C of loft drier inner drying 4h namely obtains product calcium hydrophosphate fodder through repeatedly washing; The composition of its Raw washes consists of: P
2o
5: 1% ~ 4%; SO
4: 0.002% ~ 0.01%; Ca:0.001% ~ 0.005%; F:0.0005% ~ 0.001%, the heavy metal content such as As are less than 0.0001%.
Beneficial effect of the present invention: utilize method described in this patent to prepare calcium hydrophosphate fodder, raw materials used is the reluctant phosphorous acid waste water of phosphoric acid method wood activated charcoal manufacturer, starting material belong to one of factory's " three wastes ", utilize the low phosphor resource preparation of reclaiming in waste water of this method to raise calcium product and create certain economic worth, and the mother liquor after phosphorus reclaims can use as washing active carbon water, achieve production waste zero release, what reduce gac enterprise uses water cost, resource is obtained utilize to greatest extent, while creation economic benefit, solve environmental issue again, achieve the Economic development of Enterprises formula.
Embodiment
embodiment 1
Get 1000g washes, add the polyacrylamide solution that 100g concentration is 0.1% wherein, take out after leaving standstill 6h and filter, in filtrate, add the aqua calcis of solid content 70%, control temperature of reaction 50 DEG C, reaction times 3h; Stirring velocity 300rpm, pH value 4.5, reaction terminates rear employing vacuum filtration mode and filters, and filter cake distilled water wash takes out to obtain product calcium hydrophosphate fodder after being placed on 90 DEG C of loft drier inner drying 4h for three times.Record phosphorus content 17.1% in product, calcium contents 22.4%, Oil repellent 0.023%, heavy metal content is less than 0.0001%(in As).
embodiment 2
Get 1000g washes, add the polyacrylamide solution that 100g concentration is 0.1% wherein, take out after leaving standstill 6h and filter, in filtrate, add the aqua calcis of solid content 60%, control temperature of reaction 40 DEG C, reaction times 2h; Stirring velocity 400rpm, pH value 5.0, reaction terminates rear employing vacuum filtration mode and filters, and filter cake distilled water wash takes out to obtain product calcium hydrophosphate fodder after being placed on 90 DEG C of loft drier inner drying 4h for three times.Record phosphorus content 17.8% in product, calcium contents 23.1%, Oil repellent 0.019%, heavy metal content is less than 0.0001%(in As).
embodiment 3
Get 1000g washes, add the polyacrylamide solution that 100g concentration is 0.1% wherein, take out after leaving standstill 6h and filter, in filtrate, add the aqua calcis of solid content 65%, control temperature of reaction 60 DEG C, reaction times 2h; Stirring velocity 200rpm, pH value 5.5, reaction terminates rear employing vacuum filtration mode and filters, and filter cake distilled water wash takes out to obtain product calcium hydrophosphate fodder after being placed on 90 DEG C of loft drier inner drying 4h for three times.Record phosphorus content 16.8% in product, calcium contents 24.7%, Oil repellent 0.021%, heavy metal content is less than 0.0001%(in As).
embodiment 4
Get 1000g washes, add the polyacrylamide solution that 100g concentration is 0.1% wherein, take out after leaving standstill 6h and filter, in filtrate, add the aqua calcis of solid content 70%, control temperature of reaction 50 DEG C, reaction times 2h; Stirring velocity 200rpm, pH value 4.0, reaction terminates rear employing vacuum filtration mode and filters, and filter cake distilled water wash takes out to obtain product calcium hydrophosphate fodder after being placed on 90 DEG C of loft drier inner drying 4h for three times.Record phosphorus content 16.6% in product, calcium contents 21.8%, Oil repellent 0.029%, heavy metal content is less than 0.0001%(in As).
Claims (1)
1. the washes utilizing activated carbon of phosphoric acid method to produce prepares a method for calcium hydrophosphate fodder, it is characterized in that this preparation technology is mainly divided into four processing steps: 1. pre-treatment; 2. Reactive Synthesis; 3. filter; 4. product drying;
Be specially: with the washes produced in phosphoric acid method wood activated charcoal production process for raw material, 1. pre-treatment, first the settling aids polyacrylamide solution adopted carries out pre-treatment to washes, and raw material removes the black activity charcoal powder particle trickle in a large number often contained in washes after pretreatment; 2. Reactive Synthesis, adds a certain amount of aqua calcis and carries out Reactive Synthesis, by a step neutralization reaction, prepares calcium hydrophosphate fodder product; Concrete technology parameter is: get a certain amount of washes, add the polyacrylamide solution that a certain amount of mass concentration is 0.1% wherein, make the mass concentration of polyacrylamide in solution 0.01% ~ 0.05%, filter after leaving standstill 6h, the aqua calcis of a certain amount of solid content 60% ~ 70% is added in filtrate, control temperature of reaction 40 DEG C ~ 60 DEG C, reaction times 1 h ~ 3h; Stirring velocity 150rpm ~ 400rpm, pH value 4 ~ 6, until reaction terminates; 3. filter, adopt vacuum filtration mode to filter; 4. product drying, filter cake is placed on 90 DEG C of loft drier inner drying 4h namely obtains product calcium hydrophosphate fodder through repeatedly washing; The composition of its Raw washes consists of: P
2o
5: 1% ~ 4%; SO
4: 0.002% ~ 0.01%; Ca:0.001% ~ 0.005%; F:0.0005% ~ 0.001%, the heavy metal content such as As are less than 0.0001%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410595601.1A CN104276562A (en) | 2014-10-30 | 2014-10-30 | Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410595601.1A CN104276562A (en) | 2014-10-30 | 2014-10-30 | Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104276562A true CN104276562A (en) | 2015-01-14 |
Family
ID=52251981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410595601.1A Pending CN104276562A (en) | 2014-10-30 | 2014-10-30 | Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104276562A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59207818A (en) * | 1983-05-09 | 1984-11-26 | Toyo Sutoufuaa Chem:Kk | Production of anhydrous calcium secondary phosphate of high purity |
| CN102502553A (en) * | 2011-09-30 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for preparing feed grade calcium hydrogen phosphate from waste water of phosphate fertilizer plant |
| CN103523951A (en) * | 2013-10-10 | 2014-01-22 | 徐州天正活性炭厂 | Waste water treatment technology in phosphoric acid-method active carbon production |
| CN103864469A (en) * | 2014-03-28 | 2014-06-18 | 瓮福（集团）有限责任公司 | Method for preparing feed-grade calcium hydrophosphate by using iron phosphate crystallization mother liquor |
-
2014
- 2014-10-30 CN CN201410595601.1A patent/CN104276562A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59207818A (en) * | 1983-05-09 | 1984-11-26 | Toyo Sutoufuaa Chem:Kk | Production of anhydrous calcium secondary phosphate of high purity |
| CN102502553A (en) * | 2011-09-30 | 2012-06-20 | 瓮福（集团）有限责任公司 | Method for preparing feed grade calcium hydrogen phosphate from waste water of phosphate fertilizer plant |
| CN103523951A (en) * | 2013-10-10 | 2014-01-22 | 徐州天正活性炭厂 | Waste water treatment technology in phosphoric acid-method active carbon production |
| CN103864469A (en) * | 2014-03-28 | 2014-06-18 | 瓮福（集团）有限责任公司 | Method for preparing feed-grade calcium hydrophosphate by using iron phosphate crystallization mother liquor |
Non-Patent Citations (1)
| Title |
|---|
| 张光华: "《水处理化学品》", 31 January 2005, article "有机阴离子絮凝剂原料及中间体", pages: 150-151 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102336915B (en) | Method for producing humate from base alkaline waste liquid | |
| CN103432987B (en) | Preparation method of modified kieselguhr water purifying agent | |
| CN102951723A (en) | Method for catalyzing H2O2 processing of phenol in waste water by Schwertmannite | |
| CN104193136A (en) | Method for improving sludge dewatering performance through organic acid pretreatment | |
| CN105236375A (en) | Method for preparing hydrated hydroxyl ferric phosphates by utilizing waste phosphatization slag for extraction | |
| CN105197926A (en) | Method for preparing activated carbon with enzymatic hydrolysis lignin as raw material | |
| CN102583367A (en) | Preparation technology of mesopore-rich active carbon with high specific surface area | |
| CN104338728A (en) | Biomass wet detoxification method of hexavalent chromium-contained waste residues | |
| CN103131023A (en) | Humic acid extraction novel process | |
| CN104193135A (en) | Deep dewatering method for sludge | |
| Li et al. | Biochar derived from Chinese herb medicine residues for rhodamine B dye adsorption | |
| CN105536698A (en) | Preparation method of papermaking sludge activated biochar | |
| CN104058516B (en) | A kind for the treatment of process of the phosphorus-containing wastewater in glyphosate production process generation | |
| CN105417616B (en) | The method that organic wastewater is handled with industrial residue manganese dioxide | |
| CN104878653B (en) | Preparation method for recycled paper stickies control agent | |
| CN103861566A (en) | Preparation method of efficiently-adsorptive modified starch microspheres and application of modified starch microspheres | |
| CN103539116A (en) | Process for producing activated carbon by means of phosphoric acid method | |
| CN102363580A (en) | Method for preparing phosphate fertilizer by using sewage residue of phosphate fertilizer plant | |
| CN104692837A (en) | Method of comprehensively utilizing sludge | |
| CN104276562A (en) | Method for preparing feed-grade calcium hydrogen phosphate by using washing wastewater produced by phosphoric acid process activated carbon | |
| CN103011230B (en) | Low-cost method for preparing nano calcium sulfate | |
| CN108129290B (en) | Method for removing sulfate radical in lactic acid | |
| CN101733078A (en) | Method for preparing phosphorous-removing adsorbent by using cane shoots leaves | |
| CN103599750A (en) | Preparation method porous carbon for efficiently adsorbing chrome ions in water | |
| CN113548786A (en) | Novel sludge dehydrating agent and using method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150114 |