CN113816349A - Method for synthesizing phosphorus pentafluoride by using fluorine-containing waste - Google Patents
Method for synthesizing phosphorus pentafluoride by using fluorine-containing waste Download PDFInfo
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- CN113816349A CN113816349A CN202111236882.8A CN202111236882A CN113816349A CN 113816349 A CN113816349 A CN 113816349A CN 202111236882 A CN202111236882 A CN 202111236882A CN 113816349 A CN113816349 A CN 113816349A
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
Abstract
The invention provides a method for synthesizing phosphorus pentafluoride by using fluorine-containing waste, belonging to the field of recycling of fluorine-containing waste. The method reasonably treats fluorine-containing waste generated in glass treatment by semiconductor integrated circuit manufacturing and hydrofluoric acid etching, and recycles and synthesizes phosphorus pentafluoride so as to be used for synthesizing lithium hexafluorophosphate which is a new energy product. The method changes waste into valuable, reduces the environmental pollution, expands the sources of the synthetic raw materials of the phosphorus pentafluoride and the lithium hexafluorophosphate, reduces the production cost, reduces the fluorine content in the waste water and the waste residue discharged after the treatment, reaches the national standard, and avoids causing serious environmental pollution.
Description
Technical Field
The invention belongs to the field of recycling of fluorine-containing wastes, relates to a phosphorus pentafluoride synthesis technology, and particularly relates to a method for synthesizing phosphorus pentafluoride by using fluorine-containing wastes.
Background
At present, the semiconductor integrated circuit industry in China is developed vigorously, and with the continuous expansion of the manufacturing scale, a large amount of fluorine-containing waste is generated in the production process, so that the serious pollution risk to the environment exists. The fluorine-containing waste can cause pollution to the environment and harm human health due to improper treatment. Most of the existing fluorine-containing waste residues are subjected to biochemical treatment or incineration, secondary pollutants generated are discharged in a liquid state up to the standard or buried in a solid state, and secondary pollution is generated and further the environment is seriously damaged due to improper treatment in an intermediate link. Therefore, it is important to treat the fluorine-containing waste without pollution, reduce the environmental pollution and ecological damage caused by unnecessary discharge, and reduce the possible adverse effects on animals, plants and human bodies. In addition, hydrofluoric acid etching is a commonly used method for thinning glass, and mixed acid containing hydrofluoric acid reacts with silicon dioxide and other metal oxides in glass to quickly thin the glass. The method can generate a large amount of fluorine-containing acid liquor and some insoluble metal oxides in the etching waste liquid of the thinned glass. The method for treating the fluorine-containing glass etching waste liquid at present adopts lime to treat the waste liquid, but the method has low conversion rate of hydrogen fluoride in the waste liquid, generates a large amount of mixed solids in the treatment process, needs great subsequent treatment cost, is not reasonably utilized, and belongs to resource waste.
Therefore, how to effectively recycle the fluorine-containing waste, change the fluorine-containing waste into valuable and reduce the environmental pollution is an urgent problem to be solved.
Disclosure of Invention
The invention aims to solve the problems that the conventional fluorine-containing waste is difficult to effectively utilize, so that resources are wasted and the environment is polluted, and provides a method for synthesizing phosphorus pentafluoride by utilizing the fluorine-containing waste.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the method for synthesizing the phosphorus pentafluoride by utilizing the fluorine-containing waste comprises the following steps:
(1) adding calcium silicate into the fluorine-containing glass etching waste liquid, reacting for a period of time, adding into a saturated salt solution, adding an acid solution to adjust the pH value to generate a precipitate, filtering, and collecting filter residues;
(2) adjusting the pH value of fluorine-containing waste residue water collected in the semiconductor manufacturing process to be alkaline, adding a treating agent B, stirring for reaction, filtering, and collecting filter residues;
(3) uniformly mixing the filter residue obtained in the step (1) with the filter residue obtained in the step (2), adding the obtained mixture into a reactor, adding phosphorus pentachloride into a sublimator, introducing a mixed gas of chlorine and hydrogen fluoride gas into the sublimator, heating the sublimator to sublimate the phosphorus pentachloride, and introducing the gas in the sublimator into the reactor for reaction;
(4) and (3) pressurizing and condensing the gas generated after the reaction, and rectifying and purifying to obtain the phosphorus pentafluoride.
Further, in the step (1), the addition amount of calcium silicate is 0.4-0.6 times of hydrofluoric acid in the fluorine-containing glass etching waste liquid, and the reaction time is 3-4 hours.
Further, the saturated salt solution in step (1) includes, but is not limited to, a saturated sodium chloride solution, a saturated calcium chloride solution, a saturated sodium sulfate solution, a saturated potassium sulfate solution, and a saturated potassium chloride solution.
Further, the acid solution in the step (1) is sulfuric acid, and the pH value is adjusted to 4-6.
Further, the treating agent B is calcium hydroxide, and the mass ratio of the treating agent B to fluorine ions in the fluorine-containing waste residue water is 2-3: 1.
Further, in the step (2), the pH is adjusted to 10-12, and the reaction lasts for 1-3 h.
Further, the temperature in the reactor in the step (3) is controlled to be 90-350 ℃.
Further, pressurizing to 1-1.5 MPa in the step (4).
Further, in the step (4), the temperature is condensed to 0-30 ℃.
In conclusion, the beneficial technical effects of the invention are as follows: the fluorine-containing waste generated in the glass is subjected to semiconductor integrated circuit manufacturing and hydrofluoric acid etching treatment to be recycled to synthesize phosphorus pentafluoride, so that waste is changed into valuable, the environmental pollution is reduced, the sources of raw materials for synthesizing phosphorus pentafluoride and lithium hexafluorophosphate are expanded, the production cost is reduced, the fluorine content in waste water and waste residues discharged after treatment is reduced, the national standard is met, and the serious environmental pollution is avoided.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The method for synthesizing the phosphorus pentafluoride by utilizing the fluorine-containing waste comprises the following steps:
(1) adding calcium silicate into the fluorine-containing glass etching waste liquid, reacting for a period of time, adding into a saturated salt solution, adding an acid solution to adjust the pH value to generate a precipitate, filtering, and collecting filter residues.
The fluorine-containing glass etching waste liquid contains a large amount of hydrofluoric acid, calcium fluoride precipitate and silicon tetrafluoride can be generated after calcium silicate is added, silicon tetrafluoride and hydrofluoric acid continue to react to generate fluosilicic acid, fluosilicic acid and saturated salt solution react to generate fluosilicate, the fluosilicate is insoluble in acid, and filter residue mainly contains calcium fluoride and fluosilicate.
When the fluorine-containing glass etching waste liquid is treated, the content of fluorine ions in hydrofluoric acid is measured in advance by adopting a chemical titration method, and the adding amount of calcium silicate, saturated salt solution and acid liquid is determined according to the content of the fluorine ions; the adding amount of calcium silicate is 0.4-0.6 times of that of hydrofluoric acid in the fluorine-containing glass etching waste liquid, and the reaction time is 3-4 hours; the saturated salt solution includes, but is not limited to, a saturated sodium chloride solution, a saturated calcium chloride solution, a saturated sodium sulfate solution, a saturated potassium chloride solution; the acid solution is sulfuric acid, and the pH value is adjusted to be 4-6.
(2) Adjusting the pH value of the fluorine-containing waste residue water collected in the semiconductor manufacturing process to be alkaline, adding a treating agent B, stirring for reaction, and filtering to obtain calcium fluoride; the treating agent B is calcium hydroxide, the mass ratio of the calcium hydroxide to fluorine ions in the fluorine-containing waste residue water is 2-3: 1, the pH is adjusted to 10-12, and the reaction lasts for 1-3 hours.
And (3) the fluorine-containing waste residue water in the step (2) is a mixture of fluorine-containing waste water and fluorine-containing waste residue, the fluorine-containing waste water contains a large amount of hydrofluoric acid, sodium hydroxide is added, calcium ions and fluorine ions react to generate calcium fluoride precipitate after the calcium hydroxide is dissolved, and the main component of the fluorine-containing waste residue is calcium fluoride.
(3) And (3) uniformly mixing the filter residue obtained in the step (1) with the calcium fluoride obtained in the step (2), adding the obtained mixture into a reactor, adding phosphorus pentachloride into a sublimator, introducing a mixed gas of chlorine and hydrogen fluoride gas into the sublimator, heating the sublimator to sublimate the phosphorus pentachloride, and introducing the gas in the sublimator into the reactor for reaction. The temperature in the reactor is controlled to be 90-350 ℃.
The fluosilicate reacts with the phosphorus pentachloride to generate phosphorus pentafluoride, sodium chloride and silicon tetrafluoride.
Phosphorus pentachloride is heated to 160 ℃ and sublimated, and is partially decomposed into phosphorus trichloride and chlorine gas, and is completely decomposed into phosphorus trichloride and chlorine gas when the temperature is over 300 ℃, and phosphorus trichloride, hydrogen fluoride and chlorine gas can generate phosphorus pentafluoride and hydrogen chloride; phosphorus trichloride and hydrogen fluoride will generate phosphorus trifluoride, and phosphorus trifluoride will react with chlorine and calcium fluoride to generate phosphorus pentafluoride and calcium chloride.
(4) Pressurizing and condensing the gas generated after the reaction, and rectifying and purifying to obtain phosphorus pentafluoride; wherein the pressure is increased to 1 to 1.5MPa, and the mixture is condensed to 0 to 30 ℃ in a condenser at the temperature of between 85 ℃ below zero and 60 ℃ below zero.
The phosphorus pentafluoride crude gas generated in the reaction also contains gases such as chlorine, hydrogen fluoride, hydrogen chloride and the like, the phosphorus pentafluoride is obtained by pressurization, condensation and rectification and purification, the separated chlorine and hydrogen fluoride can be recycled, and the hydrogen chloride can be recycled as a catalyst in the reaction of fluosilicate and phosphorus pentachloride.
Example 1
The content of the hydrogen fluoride in the fluorine-containing glass etching waste liquid is generally 194-1980mg/L, and the content of the hydrogen fluoride in the fluorine-containing waste water collected in the semiconductor manufacturing process is generally about 500 mg/L.
(1) Adding calcium silicate into the fluorine-containing glass etching waste liquid, reacting for a period of time, adding into a saturated salt solution, adding an acid solution to adjust the pH value to generate a precipitate, filtering, and collecting filter residues; wherein the adding amount of calcium silicate is 0.4 times of hydrofluoric acid in the fluorine-containing glass etching waste liquid, and the reaction time is 3 hours; the saturated salt solution includes, but is not limited to, a saturated sodium chloride solution, a saturated calcium chloride solution, a saturated sodium sulfate solution, a saturated potassium chloride solution; the acid solution is sulfuric acid, and the pH value is adjusted to be 4-6;
(2) adjusting the pH value of fluorine-containing waste residue water collected in the semiconductor manufacturing process to be alkaline, adding a treating agent B, stirring for reaction, filtering, and collecting filter residues; the treating agent B is calcium hydroxide, and the mass ratio of the treating agent B to fluorine ions in the fluorine-containing waste residue water is 2: 1; adjusting the pH value to 10-12, and reacting for 1 h; adjusting pH with sodium hydroxide or sulfuric acid solution;
(3) uniformly mixing the filter residue obtained in the step (1) with the filter residue obtained in the step (2), adding the obtained mixture into a reactor, adding phosphorus pentachloride into a sublimator, introducing a mixed gas of chlorine and hydrogen fluoride gas into the sublimator, heating the sublimator to sublimate the phosphorus pentachloride, and introducing the gas in the sublimator into the reactor for reaction; the temperature in the reactor is controlled at 160 ℃;
(4) pressurizing and condensing the gas generated after the reaction, and rectifying and purifying to obtain phosphorus pentafluoride; pressurizing to 1MPa, and condensing to 0-30 ℃.
The content of hydrogen fluoride in the fluorine-containing glass etching waste liquid adopted in the embodiment is 620mg/L, and the content of hydrogen fluoride in fluorine-containing waste residue water collected in the semiconductor manufacturing process is generally 500 mg/L; the phosphorus pentafluoride obtained by detection has the purity of 99.9 percent.
Example 2
(1) Adding calcium silicate into the fluorine-containing glass etching waste liquid, reacting for a period of time, adding into a saturated salt solution, adding an acid solution to adjust the pH value to generate a precipitate, filtering, and collecting filter residues; wherein the adding amount of calcium silicate is 0.6 times of hydrofluoric acid in the fluorine-containing glass etching waste liquid, and the reaction time is 4 hours; the saturated salt solution includes, but is not limited to, a saturated sodium chloride solution, a saturated calcium chloride solution, a saturated sodium sulfate solution, a saturated potassium chloride solution; the acid solution is sulfuric acid, and the pH value is adjusted to be 6;
(2) adjusting the pH value of fluorine-containing waste residue water collected in the semiconductor manufacturing process to be alkaline, adding a treating agent B, stirring for reaction, filtering, and collecting filter residues; the treating agent B is calcium hydroxide, and the mass ratio of the treating agent B to fluorine ions in the fluorine-containing waste residue water is 3: 1; adjusting the pH value to 10-12, and reacting for 3 h; adjusting pH with sodium hydroxide or sulfuric acid solution;
(3) uniformly mixing the filter residue obtained in the step (1) with the filter residue obtained in the step (2), adding the obtained mixture into a reactor, adding phosphorus pentachloride into a sublimator, introducing a mixed gas of chlorine and hydrogen fluoride gas into the sublimator, heating the sublimator to sublimate the phosphorus pentachloride, and introducing the gas in the sublimator into the reactor for reaction; the temperature in the reactor is controlled at 300 ℃;
(4) pressurizing and condensing the gas generated after the reaction, and rectifying and purifying to obtain phosphorus pentafluoride; pressurizing to 1.5MPa, and condensing to 0-30 ℃.
The fluorine-containing glass etching waste liquid adopted in the embodiment has the hydrogen fluoride content of 1620mg/L, and the fluorine-containing waste residue water collected in the semiconductor manufacturing process generally has the hydrogen fluoride content of 500 mg/L; the phosphorus pentafluoride obtained by detection has the purity of 99.9 percent.
Example 3
Adding calcium silicate into the fluorine-containing glass etching waste liquid, reacting for a period of time, adding into a saturated salt solution, adding an acid solution to adjust the pH value to generate a precipitate, filtering, and collecting filter residues; wherein the adding amount of calcium silicate is 0.5 times of hydrofluoric acid in the fluorine-containing glass etching waste liquid, and the reaction time is 3.5 h; the saturated salt solution includes, but is not limited to, a saturated sodium chloride solution, a saturated calcium chloride solution, a saturated sodium sulfate solution, a saturated potassium chloride solution; the acid solution is sulfuric acid, and the pH value is adjusted to be 5;
(2) adjusting the pH value of fluorine-containing waste residue water collected in the semiconductor manufacturing process to be alkaline, adding a treating agent B, stirring for reaction, filtering, and collecting filter residues; the treating agent B is calcium hydroxide, and the mass ratio of the treating agent B to fluorine ions in the fluorine-containing waste residue water is 2.5: 1; adjusting the pH value to 10-12, and reacting for 2 h; adjusting pH with sodium hydroxide or sulfuric acid solution;
(3) uniformly mixing the filter residue obtained in the step (1) with the filter residue obtained in the step (2), adding the obtained mixture into a reactor, adding phosphorus pentachloride into a sublimator, introducing a mixed gas of chlorine and hydrogen fluoride gas into the sublimator, heating the sublimator to sublimate the phosphorus pentachloride, and introducing the gas in the sublimator into the reactor for reaction; the temperature in the reactor is controlled at 200 ℃;
(4) pressurizing and condensing the gas generated after the reaction, and rectifying and purifying to obtain phosphorus pentafluoride; pressurizing to 1.2MPa, and condensing to 0-30 ℃.
The content of hydrogen fluoride in the fluorine-containing glass etching waste liquid adopted in the embodiment is 1120mg/L, and the content of hydrogen fluoride in fluorine-containing waste residue water collected in the semiconductor manufacturing process is generally 500 mg/L; the phosphorus pentafluoride obtained by detection has the purity of 99.9 percent.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; based on the embodiments of the present invention, a person skilled in the art may modify the technical solutions described in the foregoing embodiments without creative efforts, or may substitute part of the technical features of the embodiments; however, such modifications and substitutions do not substantially depart from the spirit and scope of the present invention, and are intended to be included within the scope thereof.
Claims (9)
1. The method for synthesizing phosphorus pentafluoride by using the fluorine-containing waste is characterized by comprising the following steps of:
(1) adding calcium silicate into the fluorine-containing glass etching waste liquid, reacting for a period of time, adding into a saturated salt solution, adding an acid solution to adjust the pH value to generate a precipitate, filtering, and collecting filter residues;
(2) adjusting the pH value of fluorine-containing waste residue water collected in the semiconductor manufacturing process to be alkaline, adding a treating agent B, stirring for reaction, filtering, and collecting filter residues;
(3) uniformly mixing the filter residue obtained in the step (1) with the filter residue obtained in the step (2), adding the obtained mixture into a reactor, adding phosphorus pentachloride into a sublimator, introducing a mixed gas of chlorine and hydrogen fluoride gas into the sublimator, heating the sublimator to sublimate the phosphorus pentachloride, and introducing the gas in the sublimator into the bottom in the reactor to react;
(4) and (3) pressurizing and condensing the gas generated after the reaction, and rectifying and purifying to obtain the phosphorus pentafluoride.
2. The method of claim 1, wherein: in the step (1), the addition amount of calcium silicate is 0.4-0.6 times of hydrofluoric acid in the fluorine-containing glass etching waste liquid, and the reaction time is 3-4 hours.
3. The method of claim 1, wherein: the saturated salt solution in the step (1) includes, but is not limited to, a saturated sodium chloride solution, a saturated calcium chloride solution, a saturated sodium sulfate solution, a saturated potassium sulfate solution, and a saturated potassium chloride solution.
4. The method of claim 1, wherein: the acid solution in the step (1) is sulfuric acid, and the pH value is adjusted to 4-6.
5. The method of claim 1, wherein: the treating agent B is calcium hydroxide, and the mass ratio of the treating agent B to fluorine ions in the fluorine-containing waste residue water is 2-3: 1.
6. The method of claim 1, wherein: in the step (2), the pH is adjusted to 10-12, and the reaction lasts for 1-3 h.
7. The method of claim 1, wherein: and (3) controlling the temperature in the reactor to be 90-350 ℃.
8. The method of claim 1, wherein: pressurizing to 1-1.5 MPa in the step (4).
9. The method of claim 1, wherein: condensing to 0-30 ℃ in the step (4).
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| CN115283422A (en) * | 2022-07-21 | 2022-11-04 | 上海市政工程设计研究总院（集团）有限公司 | Treatment method of glass etching waste residue |
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