CN1212962A - Method for producing calcium hydrogen phosphate by recovery and using waste water containing phosphate of quinacridineone serial pigment - Google Patents
Method for producing calcium hydrogen phosphate by recovery and using waste water containing phosphate of quinacridineone serial pigment Download PDFInfo
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- CN1212962A CN1212962A CN 97108251 CN97108251A CN1212962A CN 1212962 A CN1212962 A CN 1212962A CN 97108251 CN97108251 CN 97108251 CN 97108251 A CN97108251 A CN 97108251A CN 1212962 A CN1212962 A CN 1212962A
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- chemical reaction
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- auxiliary agent
- phosphate
- waste water
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B3/00—Fertilisers based essentially on di-calcium phosphate
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
A process for producing calcium hydrogen phosphate with the P-containing waste water generated during preparation of quinacridone series of dyes features that chemical neutralization reaction is used to separate phosphoric acid from the waste water, and the phosphoric acid is directly used to prepare calcium hydrogen phosphate as fertilizer. Its advantages include high fertility, cyclic use of water, high recovery rate and no secondary pollution.
Description
The present invention belongs to the field of phosphate fertilizer producing technology from waste water.
At present, phosphoric acid-containing wastewater discharged in the production process of quinacridone high-grade organic pigments runs off, so that serious pollution is caused on one hand, and effective components of the wastewater are not comprehensively utilized, so that resources are wasted.
The invention aims to provide a method for producing calcium hydrophosphate by recycling phosphorus-containing wastewater of quinacridone series pigments. The phosphate fertilizer product is prepared by recycling the phosphoric acid, the fertilizer efficiency of the phosphate fertilizer exceeds or is equivalent to that of other phosphate fertilizers, and the waste water is recycled for closed circulation.
The invention is realized by the following modes: the method is characterized in that an acid-base neutralization method is adopted, CaO (lime or calcium carbide waste residue) is used as a raw material to generate calcium phosphate salts with different solubilities, and crystalline precipitates are generated under a determined control condition to facilitate separation; the chemical reaction formula is as follows:
The invention has the following advantages: 1. the invention selects CaO (lime or calcium carbide waste residue) as a raw material, separates phosphoric acid in the waste water by a neutralization reaction method, directly produces the calcium hydrophosphate fertilizer, and has simple, convenient and feasible method. 2. The process method of the invention is carried out at normal temperature and normal pressureThe method has good repeatability, good production and recovery of fertilizer phosphorus, total phosphorus and available phosphorus, and high recovery rate up to over 96%. 3. The recovered waste water contains a small amount of phosphoric acid which can be recycled, and Ca (OH) is prepared2The suspension liquid does not cause secondary pollution, realizes closed circulation, does not discharge waste water, utilizes resources, is comprehensively treated, changes waste into valuable, protects the environment and supportsagriculture. 4. Because the recycled wastewater has different components, the produced calcium hydrophosphate does not contain toxic elements and can be used as feed; the quinacridone pigment and the quinacridone pigment except the small amount of quinacridone pigment which contain a small amount of methanol meet the standard requirements of fertilizers, the quinacridone pigment is used as a phosphate fertilizer, the quinacridone pigment is a nontoxic organic pigment, the phosphate fertilizer is a qualified phosphate fertilizer, and the fertilizer effect is remarkable. The P content of the feed product is more than 16 percent, and the effective P of the phosphate fertilizer product2O5＞18-30％。
The present invention will now be described in further detail with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of the process of the present invention.
Referring to fig. 1, the chemical reaction of the present invention is carried out in a reaction vessel. The basic principle of the invention is to separate phosphate from waste water by an acid-base neutralization method, calcium phosphate salts with different solubilities can be generated by taking CaO (lime or calcium carbide waste residue) as a raw material, and a crystal type precipitate is generated under certain control conditions, so that the separation is convenient. The calcium hydrogen phosphate precipitate is citrate soluble available phosphorus with available P2O5The highest content can reach more than 30 percent, and the fertilizer is a good agricultural phosphate fertilizer. Two kinds of phosphorus-containing wastewater are discharged in the quinacridone pigment production process according to different products, wherein one kind of wastewaterdoes not contain methanol, and the other kind of wastewater contains methanol. The former can be directly used for recycling and producing phosphate fertilizer through the chemical reaction of the reaction kettle, and the latter must be used for recycling methanol through the distillation tower and then enter the reaction kettle for recycling and producing phosphate fertilizer through the chemical reaction. The above-mentioned certain amount of waste water and Ca (OH) -containing water2A suspension of (a). And the auxiliary agent reacts under the controlled condition to generate calcium hydrophosphate precipitate, the phosphate fertilizer product is obtained after filtration and precipitate drying, and the filtrate is recycled for preparing Ca (OH)2. MiningBy CaHPO4Or SiO2Or Ca3(PO4)2As an auxiliary agent, a proper amount of the phosphate is added, so that the phosphate is precipitated and separated, and the separation process has good effect. In the raw material preparation, quicklime (or calcium carbide waste residue) is added into the circulating filtrate, and the mixture is stirred to prepare suspension. Is pumped intoStirring the mixture in a reaction kettle filled with a certain amount of waste water, and directly reacting phosphoric acid in the waste water with Ca (OH) under the conditions of normal temperature and normal pressure and control2The reaction produces crystalline calcium hydrogen phosphate.
The production conditions were controlled as follows: normal temperature and pressure, temperature of 35-65 deg.C
The pH value is 5-7
The drying temperature is 80-100 ℃.
Claims (1)
1. A method for producing calcium hydrophosphate by recycling phosphorus-containing wastewater of quinacridone series pigments is characterized by comprising the following steps: the method adopts an acid-base neutralization method to separate phosphate from the phosphorus-containing wastewater, takes CaO (lime or calcium carbide waste residues) as a raw material to generate calcium phosphate salts with different solubilities, and generates crystalline precipitates under a determined control condition so as to be convenient for separation; the chemical reaction formula is as follows: the process flow is as follows:
(1) the phosphoric acid wastewater containing methanol enters a chemical reaction after the methanol is recovered and distilled out, wherein the chemical reaction is generated by adding Ca (OH)2 and an auxiliary agent, and the chemical reaction formula is the 2 formulas; precipitating, separating and drying the product after the chemical reaction, and returning the filtrate into Ca (OH)2 and the auxiliary agent for the chemical reaction; recycling; drying, analyzing and testing the precipitate to obtain a product;
(2) the phosphoric acid wastewater without methanol directly enters into a chemical reaction, and the chemical reaction is also generated by adding Ca' (OH)2 and an auxiliary agent, and the chemical reaction formula is the 2 formulas; precipitating, separating and drying the product after the chemical reaction, returning the filtrate into Ca (OH)2 and the auxiliary agent for the chemical reaction and recycling; the precipitate is dried, analyzed and assayed to obtain the product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97108251A CN1064651C (en) | 1997-09-29 | 1997-09-29 | Method for producing calcium hydrogen phosphate by recovery and using waste water containing phosphate of quinacridineone serial pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97108251A CN1064651C (en) | 1997-09-29 | 1997-09-29 | Method for producing calcium hydrogen phosphate by recovery and using waste water containing phosphate of quinacridineone serial pigment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1212962A true CN1212962A (en) | 1999-04-07 |
| CN1064651C CN1064651C (en) | 2001-04-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97108251A Expired - Fee Related CN1064651C (en) | 1997-09-29 | 1997-09-29 | Method for producing calcium hydrogen phosphate by recovery and using waste water containing phosphate of quinacridineone serial pigment |
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| CN (1) | CN1064651C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD3978C2 (en) * | 2009-02-04 | 2010-06-30 | Государственный Университет Молд0 | Process for dephosphatation of sewage waters |
| CN102225826A (en) * | 2011-05-10 | 2011-10-26 | 浙江永泉化学有限公司 | Decolorization and phosphorus reduction method for high-concentration phosphorus-containing wastewater from quinacridone pigment production process |
| CN109293058A (en) * | 2018-10-26 | 2019-02-01 | 洪湖市泰科技有限公司 | A kind of method of phosphorus-containing wastewater recycled and waste resource recovery utilizes |
| CN110885122A (en) * | 2019-11-30 | 2020-03-17 | 怀化恒一颜料化学有限公司 | Process for treating waste water from quinacridone production |
| CN110885125A (en) * | 2019-12-02 | 2020-03-17 | 怀化恒一颜料化学有限公司 | Quinacridone production wastewater treatment equipment |
| CN112062348A (en) * | 2020-09-14 | 2020-12-11 | 怀化恒一颜料化学有限公司 | Quinacridone pigment waste water processing system |
| CN114249452A (en) * | 2020-09-25 | 2022-03-29 | 怀化恒一颜料化学有限公司 | Method for recovering phosphoric acid from quinacridone production wastewater |
| CN114684967A (en) * | 2022-04-06 | 2022-07-01 | 深圳大学 | Synergistic treatment method for calcareous solid waste and phosphorus-containing waste liquid and application of product thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4988489A (en) * | 1989-01-25 | 1991-01-29 | Todd Lanny E | Recovery of phosphorus values from waste phosphoric acid liquors |
-
1997
- 1997-09-29 CN CN97108251A patent/CN1064651C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD3978C2 (en) * | 2009-02-04 | 2010-06-30 | Государственный Университет Молд0 | Process for dephosphatation of sewage waters |
| CN102225826A (en) * | 2011-05-10 | 2011-10-26 | 浙江永泉化学有限公司 | Decolorization and phosphorus reduction method for high-concentration phosphorus-containing wastewater from quinacridone pigment production process |
| CN109293058A (en) * | 2018-10-26 | 2019-02-01 | 洪湖市泰科技有限公司 | A kind of method of phosphorus-containing wastewater recycled and waste resource recovery utilizes |
| CN110885122A (en) * | 2019-11-30 | 2020-03-17 | 怀化恒一颜料化学有限公司 | Process for treating waste water from quinacridone production |
| CN110885125A (en) * | 2019-12-02 | 2020-03-17 | 怀化恒一颜料化学有限公司 | Quinacridone production wastewater treatment equipment |
| CN112062348A (en) * | 2020-09-14 | 2020-12-11 | 怀化恒一颜料化学有限公司 | Quinacridone pigment waste water processing system |
| CN114249452A (en) * | 2020-09-25 | 2022-03-29 | 怀化恒一颜料化学有限公司 | Method for recovering phosphoric acid from quinacridone production wastewater |
| CN114684967A (en) * | 2022-04-06 | 2022-07-01 | 深圳大学 | Synergistic treatment method for calcareous solid waste and phosphorus-containing waste liquid and application of product thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1064651C (en) | 2001-04-18 |
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