CN111847413A - Method for preparing trisodium phosphate by using phosphoric acid-containing waste material - Google Patents
Method for preparing trisodium phosphate by using phosphoric acid-containing waste material Download PDFInfo
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- CN111847413A CN111847413A CN202010579460.XA CN202010579460A CN111847413A CN 111847413 A CN111847413 A CN 111847413A CN 202010579460 A CN202010579460 A CN 202010579460A CN 111847413 A CN111847413 A CN 111847413A
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 239000002699 waste material Substances 0.000 title claims abstract description 51
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 48
- 239000001488 sodium phosphate Substances 0.000 title claims abstract description 40
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 title claims abstract description 40
- 229910000406 trisodium phosphate Inorganic materials 0.000 title claims abstract description 40
- 235000019801 trisodium phosphate Nutrition 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000011259 mixed solution Substances 0.000 claims abstract description 62
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 238000004062 sedimentation Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- -1 molybdenum ion Chemical class 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000012452 mother liquor Substances 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 239000010413 mother solution Substances 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 description 13
- 239000007788 liquid Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 230000008901 benefit Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000003814 drug Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 150000001447 alkali salts Chemical class 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910013885 M3(PO4)2 Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 231100000171 higher toxicity Toxicity 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/305—Preparation from phosphorus-containing compounds by alkaline treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention discloses a method for preparing trisodium phosphate by using phosphoric acid-containing waste materials, which comprises the following steps: subjecting the phosphoric acid-containing waste to distillation treatment; adding a first alkaline reagent to the phosphoric acid-containing waste subjected to the distillation treatment to form a first mixed solution; sequentially carrying out first sedimentation treatment and first filtration treatment on the first mixed solution to obtain a second mixed solution; adding a second alkaline reagent to the second mixed solution to form a third mixed solution; sequentially carrying out second sedimentation treatment and second filtration treatment on the third mixed solution to obtain a fourth mixed solution; adding a sodium hydroxide solution into the fourth mixed solution and carrying out reaction treatment to obtain a fifth mixed solution; post-treating the fifth mixed solution to obtain the trisodium phosphate. During the whole process, trisodium phosphate with the purity of more than 97 percent can be prepared, and the harmless treatment and resource utilization of the phosphoric acid-containing waste are realized.
Description
Technical Field
The invention belongs to the technical field of harmless treatment and resource utilization of wastes, and particularly relates to a method for preparing trisodium phosphate by using phosphoric acid-containing wastes.
Background
In chemical etchingIn the industrial production process of electrochemical polishing and the like, for example, aluminum products need a polishing process, and a polishing agent usually adopts a mixed solution prepared by proportioning phosphoric acid, so that phosphoric acid waste containing metal and other impurities is generated in the production process of enterprises. The waste acid pollutants are mainly H-Metal ions and various acid radicals, and the wastewater is acidic and can not be biochemically generated. The waste acid produced by the production has high concentration of pollutants and higher toxicity, and is easy to cause resource waste after being treated according to the traditional waste acid.
At present, two main processes for treating waste phosphoric acid are industrially available: recovering acid, salt and the like; for example, the waste phosphoric acid solution is added with at least one oxide to react: 2H3PO4+3MO＝M3(PO4)2↓+3H2And O, then discharging the waste water after solid-liquid separation so as to recycle the phosphoric acid. For another example, industrial sulfates and hydrogenphosphates are obtained by removing impurities, primary sedimentation, neutralization, secondary sedimentation, plate-and-frame filter pressing and mixing filter residues.
However, the current method for preparing trisodium phosphate by using phosphoric acid-containing waste materials still needs to be further improved.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a method for preparing trisodium phosphate by using phosphoric acid-containing waste, which adopts a distillation impurity removal process, a medicament impurity removal process, an alkali salt preparation process, a solid-liquid separation process and a mother liquor refining process to cooperatively treat the phosphoric acid-containing waste (the main component is H) -Metal ions and various acid radical waste acid solutions). Mainly solves at least one of the following problems existing at present: (1) the conventional method for treating the waste material containing phosphoric acid causes the waste of phosphoric acid; (2) the recovery cost of phosphoric acid prepared from phosphoric acid-containing waste materials is high; (3) the difficulty of preparing high-purity phosphate from the phosphoric acid-containing waste is high.
The purpose of the invention is realized by the following technical scheme:
a method for preparing trisodium phosphate from phosphoric acid-containing waste material, comprising the steps of:
subjecting the phosphoric acid-containing waste to distillation treatment;
adding a first alkaline reagent to the phosphoric acid-containing waste subjected to the distillation treatment to form a first mixed solution;
sequentially carrying out first sedimentation treatment and first filtration treatment on the first mixed solution to obtain a second mixed solution;
adding a second alkaline reagent to the second mixed solution to form a third mixed solution;
sequentially carrying out second sedimentation treatment and second filtration treatment on the third mixed solution to obtain a fourth mixed solution;
adding a sodium hydroxide solution into the fourth mixed solution and carrying out reaction treatment to obtain a fifth mixed solution;
post-treating the fifth mixed solution to obtain the trisodium phosphate.
According to an embodiment of the invention, based on the total mass of the phosphoric acid-containing waste, the content of phosphoric acid is 60-90 wt%, the content of acetic acid is 6-10 wt%, the content of nitric acid is 1-5 wt%, the content of molybdenum ions is 0.1-0.5 wt%, and the content of aluminum ions is 1-5 wt%.
According to the specific embodiment of the invention, the temperature of the distillation treatment is 120-160 ℃, and the time is 1-5 hours.
According to a particular embodiment of the invention, the first alkaline agent is solid sodium carbonate; and/or the pH value of the first mixed solution is 1-5.
According to a particular embodiment of the invention, the second alkaline agent is solid sodium hydroxide; and/or the pH value of the third mixed solution is 6-9.
According to an embodiment of the invention, the pH of the fifth mixed solution is 11-13.
According to a specific embodiment of the present invention, the post-processing comprises:
conveying the fifth mixed solution to a crystallization tank, stirring and cooling the fifth mixed solution to separate out a first crude trisodium phosphate product, and separating the first crude trisodium phosphate product from a mother solution by using a centrifuge;
refining the mother liquor to obtain a second trisodium phosphate crude product;
wherein, the purity of the first trisodium phosphate crude product is not lower than 97 percent;
The purity of the second trisodium phosphate crude product is not lower than 97%;
the first and second crude trisodium phosphate products comprise the trisodium phosphate.
According to the specific embodiment of the invention, the content of the acetic acid is not higher than 0.3 wt% and the content of the nitric acid is not higher than 0.08 wt% based on the total mass of the phosphoric acid-containing waste material subjected to the distillation treatment.
According to a specific embodiment of the present invention, the content of the molybdenum ion is not more than 0.01 wt% based on the total mass of the first mixed solution.
According to a specific embodiment of the present invention, the content of the aluminum ions is not higher than 0.1 wt% based on the total mass of the third mixed solution.
The treatment effect of the invention is as follows: the invention prepares trisodium phosphate by using phosphoric acid-containing waste, adopts the distillation impurity removal medicament for impurity removal and the refining process of the alkali-added salt-making solid-liquid separation mother liquor for synergistic treatment, and has at least one of the following advantages: the method has the characteristics of stable operation, convenient management, high salt production purity, stable yield and the like, can greatly improve the resource utilization rate of the phosphoric acid-containing waste materials in production and application, realizes the harmless treatment and resource utilization of the phosphoric acid-containing waste liquid, reduces the pollution to the environment, achieves the purpose of recycling the waste materials, and has good environmental benefit and social benefit.
Drawings
FIG. 1 is a block diagram of a specific process for preparing trisodium phosphate from phosphoric acid-containing waste material according to the present invention.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
The invention provides a method for preparing high-purity trisodium phosphate by using waste phosphoric acid, which comprises the following steps:
subjecting the phosphoric acid-containing waste to distillation treatment;
adding a first alkaline reagent to the phosphoric acid-containing waste subjected to the distillation treatment to form a first mixed solution;
sequentially carrying out first sedimentation treatment and first filtration treatment on the first mixed solution to obtain a second mixed solution;
adding a second alkaline reagent to the second mixed solution to form a third mixed solution;
sequentially carrying out second sedimentation treatment and second filtration treatment on the third mixed solution to obtain a fourth mixed solution;
adding a sodium hydroxide solution into the fourth mixed solution and carrying out reaction treatment to obtain a fifth mixed solution;
post-treating the fifth mixed solution to obtain the trisodium phosphate.
According to an embodiment of the invention, based on the total mass of the phosphoric acid-containing waste, the content of phosphoric acid is 60-90 wt%, the content of acetic acid is 6-10 wt%, the content of nitric acid is 1-5 wt%, the content of molybdenum ions is 0.1-0.5 wt%, and the content of aluminum ions is 1-5 wt%.
According to the specific embodiment of the invention, the temperature of the distillation treatment is 120-160 ℃, and the time is 1-5 hours.
According to a particular embodiment of the invention, the first alkaline agent is solid sodium carbonate.
According to the specific embodiment of the invention, the pH of the first mixed solution is 1-5.
According to a particular embodiment of the invention, the second alkaline agent is solid sodium hydroxide.
According to the specific embodiment of the invention, the pH of the third mixed solution is 6-9.
According to an embodiment of the invention, the pH of the fifth mixed solution is 11-13.
According to a specific embodiment of the present invention, the post-processing comprises:
conveying the fifth mixed solution to a crystallization tank, stirring and cooling the fifth mixed solution to separate out a first crude trisodium phosphate product, and separating the first crude trisodium phosphate product from a mother solution by using a centrifuge;
refining the mother liquor to obtain a second trisodium phosphate crude product;
wherein, the purity of the first trisodium phosphate crude product is not lower than 97 percent;
the purity of the second trisodium phosphate crude product is not lower than 97%;
the first and second crude trisodium phosphate products comprise the trisodium phosphate.
According to the specific embodiment of the invention, the content of the acetic acid is not higher than 0.3 wt% and the content of the nitric acid is not higher than 0.08 wt% based on the total mass of the phosphoric acid-containing waste material subjected to the distillation treatment.
According to a specific embodiment of the present invention, the content of the molybdenum ion is not more than 0.01 wt% based on the total mass of the first mixed solution.
According to a specific embodiment of the present invention, the content of the aluminum ions is not higher than 0.1 wt% based on the total mass of the third mixed solution.
The invention prepares trisodium phosphate by using phosphoric acid-containing waste, adopts the distillation impurity removal medicament for impurity removal and the refining process of the alkali-added salt-making solid-liquid separation mother liquor for synergistic treatment, and has at least one of the following advantages: the method has the characteristics of stable operation, convenient management, high salt production purity, stable yield and the like, can greatly improve the resource utilization rate of the phosphoric acid-containing waste materials in production and application, realizes the harmless treatment and resource utilization of the phosphoric acid-containing waste liquid, reduces the pollution to the environment, achieves the purpose of recycling the waste materials, and has good environmental benefit and social benefit.
Example 1:
10.5t of phosphoric acid-containing waste is taken, and the phosphoric acid content in the raw material liquid is analyzed to be 60 percent (wt percent); the content of acetic acid is about 8 percent (wt%), the content of nitric acid is about 2 percent (wt%), the content of aluminum ions is about 2 percent (wt%), and the content of molybdenum ions is about 0.2 percent (wt%), and the distillation impurity removal, the chemical impurity removal, the alkali salt preparation, the solid-liquid separation and the mother liquor refining process are adopted to carry out the synergistic treatment as shown in figure 1.
And (3) distilling for three hours at the temperature of 120-160 ℃, wherein the content of acetic acid is reduced to 0.3% (wt%), and the content of nitric acid is reduced to 0.08% (wt%). Then, solid sodium carbonate and solid sodium hydroxide are sequentially added, and sedimentation treatment and filtration treatment are respectively carried out, after medicament impurity removal, the content of molybdenum ions is 0.01% (wt%), the content of aluminum ions is 0.1% (wt%), finally, after alkali salt preparation treatment and further post-treatment, the purity of the prepared trisodium phosphate reaches 99.3%.
The invention utilizes the distillation impurity removal and medicament impurity removal processes to produce a high-purity trisodium phosphate product, eliminates the harm of phosphoric acid-containing waste to the environment, realizes the resource utilization of waste, and improves the value of the waste. Has the advantages of stable operation, convenient management, high product purity, high yield and the like.
The above-described embodiments are intended to illustrate rather than to limit the invention, and any variations, modifications, substitutions and alterations of the present invention are intended to fall within the scope of the appended claims.
Claims (10)
1. A method for preparing trisodium phosphate by using phosphoric acid-containing waste materials is characterized by comprising the following steps:
Subjecting the phosphoric acid-containing waste to distillation treatment;
adding a first alkaline reagent to the phosphoric acid-containing waste subjected to the distillation treatment to form a first mixed solution;
sequentially carrying out first sedimentation treatment and first filtration treatment on the first mixed solution to obtain a second mixed solution;
adding a second alkaline reagent to the second mixed solution to form a third mixed solution;
sequentially carrying out second sedimentation treatment and second filtration treatment on the third mixed solution to obtain a fourth mixed solution;
adding a sodium hydroxide solution into the fourth mixed solution and carrying out reaction treatment to obtain a fifth mixed solution;
post-treating the fifth mixed solution to obtain the trisodium phosphate.
2. The method according to claim 1, wherein the content of phosphoric acid is 60 to 90 wt%, the content of acetic acid is 6 to 10 wt%, the content of nitric acid is 1 to 5 wt%, the content of molybdenum ion is 0.1 to 0.5 wt%, and the content of aluminum ion is 1 to 5 wt% based on the total mass of the phosphoric acid-containing waste material.
3. The method according to claim 2, wherein the temperature of the distillation treatment is 120 to 160 ℃ and the time is 2 to 5 hours.
4. The method according to claim 2, characterized in that the first alkaline agent is solid sodium carbonate; and/or
The pH value of the first mixed solution is 1-5.
5. The method of claim 2, wherein the second alkaline agent is solid sodium hydroxide; and/or
And the pH value of the third mixed solution is 6-9.
6. The method according to claim 1, wherein the pH of the fifth mixed solution is 11 to 13.
7. The method of claim 1, wherein the post-processing comprises:
conveying the fifth mixed solution to a crystallization tank, stirring and cooling the fifth mixed solution to separate out a first crude trisodium phosphate product, and separating the first crude trisodium phosphate product from a mother solution by using a centrifuge;
refining the mother liquor to obtain a second trisodium phosphate crude product;
wherein, the purity of the first trisodium phosphate crude product is not lower than 97 percent;
the purity of the second trisodium phosphate crude product is not lower than 97%;
the first and second crude trisodium phosphate products comprise the trisodium phosphate.
8. The method of claim 3, wherein the acetic acid content is not higher than 0.3 wt% and the nitric acid content is not higher than 0.08 wt% based on the total mass of the phosphoric acid-containing waste material subjected to the distillation treatment.
9. The method according to claim 4, wherein the content of the molybdenum ion is not higher than 0.01 wt% based on the total mass of the first mixed solution.
10. The method according to claim 5, wherein the content of the aluminum ions is not higher than 0.1 wt% based on the total mass of the third mixed solution.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831542A (en) * | 2010-04-23 | 2010-09-15 | 北京科技大学 | Method for extracting metallic elements of ferrum, magnesium and calcium from molybdenum milltailings |
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| CN105714123A (en) * | 2016-05-04 | 2016-06-29 | 中条山有色金属集团有限公司 | Method for preparing ammonium rhenate from rhenium-rich slag |
| CN106395777A (en) * | 2016-08-30 | 2017-02-15 | 湖北永绍科技股份有限公司 | Comprehensive utilization method of phosphoric acid waste liquid |
| CN109437137A (en) * | 2018-12-28 | 2019-03-08 | 湖北泰盛化工有限公司 | A kind of method that the purification of crude product sodium pyrophosphate produces tertiary sodium phosphate and sodium chloride |
| CN109809379A (en) * | 2019-03-19 | 2019-05-28 | 柯芬 | The recoverying and utilizing method of phosphorus in phosphorous waste material |
| CN110482572A (en) * | 2019-08-08 | 2019-11-22 | 湖北兴福电子材料有限公司 | A kind of classification recoverying and utilizing method of aluminium scrap etching solution |
-
2020
- 2020-06-23 CN CN202010579460.XA patent/CN111847413A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831542A (en) * | 2010-04-23 | 2010-09-15 | 北京科技大学 | Method for extracting metallic elements of ferrum, magnesium and calcium from molybdenum milltailings |
| CN103264998A (en) * | 2013-05-14 | 2013-08-28 | 湖北吉星化工集团有限责任公司 | Recycle of calcium phosphate |
| CN105714123A (en) * | 2016-05-04 | 2016-06-29 | 中条山有色金属集团有限公司 | Method for preparing ammonium rhenate from rhenium-rich slag |
| CN106395777A (en) * | 2016-08-30 | 2017-02-15 | 湖北永绍科技股份有限公司 | Comprehensive utilization method of phosphoric acid waste liquid |
| CN109437137A (en) * | 2018-12-28 | 2019-03-08 | 湖北泰盛化工有限公司 | A kind of method that the purification of crude product sodium pyrophosphate produces tertiary sodium phosphate and sodium chloride |
| CN109809379A (en) * | 2019-03-19 | 2019-05-28 | 柯芬 | The recoverying and utilizing method of phosphorus in phosphorous waste material |
| CN110482572A (en) * | 2019-08-08 | 2019-11-22 | 湖北兴福电子材料有限公司 | A kind of classification recoverying and utilizing method of aluminium scrap etching solution |
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