CN107792841B - Method for producing sodium tripolyphosphate without chloride and fluoride - Google Patents
Method for producing sodium tripolyphosphate without chloride and fluoride Download PDFInfo
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- CN107792841B CN107792841B CN201711050652.6A CN201711050652A CN107792841B CN 107792841 B CN107792841 B CN 107792841B CN 201711050652 A CN201711050652 A CN 201711050652A CN 107792841 B CN107792841 B CN 107792841B
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
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- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
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- C01B25/418—After-treatment
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Abstract
A method for producing sodium tripolyphosphate without chloride and fluoride is realized by the following steps: (1) and (3) neutralization reaction: adding water into a neutralization pot, heating, adding soda ash, stirring to completely dissolve the soda ash, slowly adding phosphoric acid while stirring when the temperature of the solution rises to 90-120 ℃, adjusting the K value of the neutralization slurry to be 2.8 +/-0.2, adding silicon dioxide, continuously reacting for 3.5 +/-0.5 h until the neutralization slurry is viscous, and filtering to obtain viscous slurry for later use; (2) drying and dehydrating: sending the neutralized viscous slurry into a drying tower for atomization and dehydration; (3) and (3) polymerization generation: carrying out polymerization reaction on the dried and dehydrated raw materials to obtain sodium tripolyphosphate; (4) and (3) carrying out alkaline washing on the tail gas containing hydrogen chloride, hydrogen fluoride and silicon tetrafluoride, and emptying after the tail gas is detected to be qualified. The production method of sodium tripolyphosphate provided by the invention has the advantages of low raw material cost, simple process, easy realization of industrialization and easy obtainment of raw materials, and the obtained sodium tripolyphosphate does not contain chloride and fluoride.
Description
Technical Field
The invention relates to a preparation method of sodium tripolyphosphate, in particular to a method for producing sodium tripolyphosphate without chloride and fluoride.
Background
Sodium tripolyphosphate is used as a softening agent, a dispersing agent and a dyeing auxiliary agent. The softener for the industrial water can reduce the content of metal ions such as calcium, magnesium, iron and the like in the industrial water and reduce the hardness of the water; the dispersant is used in industrial configuration of paint, kaolin, magnesium oxide, calcium carbonate and the like, and is used as a drilling mud dispersant. In addition, the water reducing agent can also be used as a detergent auxiliary agent, a food additive, a water reducing agent for molds such as gypsum and the like. When the water softener is applied to industrial water softening, the excessive residual quantity of chloride and fluoride can limit the next application of industrial water, and when the water softener is applied to industrial configurations such as paint, kaolin, magnesium oxide, calcium carbonate and the like, the excessive residual quantity of chloride and fluoride can influence the purity of downstream products and reduce the added value of the products. To solve this problem, sodium tripolyphosphate without chloride and fluoride is generally produced by using food-grade sodium hydroxide solution and hot phosphoric acid as raw materials. The high production costs and energy consumption limit the large-scale application of this process.
Wet phosphoric acid generally contains fluoride residues, and soda ash generally contains chloride residues. By the method disclosed by the invention, wet-process phosphoric acid and soda ash can be used as raw materials to produce sodium tripolyphosphate without chloride and fluoride.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for producing sodium tripolyphosphate without chloride and fluoride.
The purpose of the invention is realized as follows: a method for producing sodium tripolyphosphate without chloride and fluoride is realized by the following steps:
(1) and (3) neutralization reaction: preparing a soda solution with the mass concentration of 30-50%, when the temperature of the solution rises to 90-120 ℃, slowly adding solid sodium carbonate and phosphoric acid while stirring, adjusting the K value of the neutralized slurry to be 2.8 +/-0.2, controlling the specific gravity of the neutralized slurry to be 1.4-1.6, adding silicon dioxide, continuously reacting for 3.5 +/-0.5 h to be viscous, and filtering to obtain viscous slurry for later use;
(2) drying and dehydrating: sending the neutralized viscous slurry into a drying tower for atomization and dehydration;
(3) and (3) polymerization generation: carrying out polymerization reaction on the dried and dehydrated raw materials to obtain white powdery or fine particle sodium tripolyphosphate;
(4) and (3) carrying out alkaline washing on the tail gas containing hydrogen chloride, hydrogen fluoride and silicon tetrafluoride, and emptying after the tail gas is detected to be qualified.
Silicon dioxide is added into the neutralized slurry, the adding amount of the silicon dioxide is 0.1-0.5% of the mass of the phosphoric acid, and the reaction time is 3.5 +/-0.5 h. The particle size of the silicon dioxide is 50-150 mu m.
In the preferred mode, after the temperature of the soda solution is raised to 100 ℃, 85 percent phosphoric acid and solid sodium carbonate are added.
In the preferred mode, when the K value of the neutralization slurry in the mixed system is adjusted to be 2.8 +/-0.2 by adding 85% of phosphoric acid and solid sodium carbonate, the addition of the phosphoric acid is stopped, and the specific gravity of the neutralization slurry is controlled to be 1.4-1.6.
More preferably, when the K value of the neutralized slurry in the mixed system is adjusted to 2.8 + -0.1 by adding 85% phosphoric acid and solid sodium carbonate, the addition of phosphoric acid is stopped and the specific gravity of the neutralized slurry is controlled to 1.5.
The polymerization temperature in the polymerization reaction is 380-450 ℃. Further preferably, the polymerization temperature in the polymerization reaction is 420 ℃.
The sodium carbonate is in industrial grade or food grade, and the phosphoric acid is wet-process phosphoric acid with the mass concentration of 85% or hot-process phosphoric acid with the mass concentration of 85%.
The preparation method of the sodium carbonate solution in the step 1) comprises the following steps: adding water into the neutralization pot, heating to 80 ℃ by using steam, and adding solid sodium carbonate to dissolve completely to obtain the required soda solution.
In the invention, silicon dioxide is added into the neutralized slurry, the addition amount is 0.1-0.5% of the mass of phosphoric acid, and the reaction time is 3.5 +/-0.5 h. The particle size of the silicon dioxide is 50-150 mu m. The silicon dioxide mainly reacts with fluoride (mainly existing in the form of sodium fluoride) in the neutralized slurry to generate silicon tetrafluoride, and the silicon tetrafluoride steam has high partial pressure and is easy to remove. The relevant reaction equation is as follows:
SiO2+H3PO4→H2SiO3+HPO3
H3PO4+NaF→HF↑+NaH2PO4
H2SiO3+4HF→SiF4↑+3H2O
the K value of the neutralized slurry is 2.8 +/-0.2. By reducing the K value of the slurry and increasing the using amount of phosphoric acid, the conversion of fluoride and chloride is effectively promoted.
The polymerization temperature in the polymerization reaction is 380-450 ℃. The removal of the chloride and the fluoride converted into gaseous substances is effectively promoted by increasing the polymerization reaction temperature. The relevant reaction equation is as follows:
H3PO4+NaCL→HCL↑+NaH2PO4
H3PO4+NaF→HF↑+NaH2PO4
H2SiO3+4HF→SiF4↑+3H2O
compared with the traditional process, the invention has the outstanding advantages that:
(1) the invention can use raw material range to expand, the traditional process uses food grade 42% sodium hydroxide solution and thermal method phosphate as raw materials, the invention can also use industrial grade or food grade sodium carbonate and wet method phosphoric acid or thermal method phosphoric acid as raw materials.
(2) The method converts fluoride and chloride into hydrogen fluoride and hydrogen chloride by reducing the K value of the slurry; the dissipation of the hydrogen chloride and the hydrogen fluoride is facilitated by increasing the polymerization reaction temperature; and simultaneously, a small amount of silicon dioxide is added in the reaction, so that the residual fluoride is converted into silicon tetrafluoride with higher steam partial pressure. The three joint controls allow the fluoride and chloride in the feedstock to escape in gaseous form.
(3) According to the reaction equation:
6H3PO4+5Na2CO3→4Na2HPO4+2NaH2PO4+5CO2↑+5H2O
3H3PO4+5NaOH→2Na2HPO4+NaH2PO4+5H2O
NaH2PO4+2Na2HPO4→Na5P3O10+2H2O
under the condition of the same amount of phosphoric acid, 0.4mol of sodium tripolyphosphate can be obtained by 1mol of sodium carbonate; whereas 1mol of a 42% strength sodium hydroxide solution gives only 0.084mol of sodium tripolyphosphate. The method has the advantages of higher yield and lower cost.
(4) According to the invention, silicon dioxide is creatively selected to participate in the reaction, and residual hydrogen fluoride is converted into silicon tetrafluoride with higher steam partial pressure, so that the product does not contain fluoride completely. The redundant silicon dioxide is filtered in a slurry fine filtering section and is washed and recycled.
Detailed Description
Example 1
Adding 5 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 4.5 tons of industrial-grade sodium carbonate, stirring to completely dissolve the sodium carbonate, slowly adding 85 percent wet-process phosphoric acid and 3.5 tons of solid sodium carbonate under stirring when the temperature of the solution rises to 90 ℃ for reaction, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 2.6, and metering the addition amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.4, adding silicon dioxide, continuing to react for 3 hours, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 380 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
In the above reaction, silica was added in an amount of 0.1% by mass of phosphoric acid. The overall reaction process can be represented by the following equation:
6H3PO4+5Na2CO3→4Na2HPO4+2NaH2PO4+5CO2↑+5H2O
NaH2PO4+2Na2HPO4→Na5P3O10+2H2O
fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
The relevant test results are as follows:
example 2
Adding 10 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 6 tons of industrial-grade soda ash, stirring to completely dissolve the soda ash, slowly adding wet-process phosphoric acid and 7 tons of soda ash for reaction under stirring when the temperature of the solution rises to 100 ℃, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 2.8, and metering the adding amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.5, adding silicon dioxide, continuing to react for 3.5h, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 400 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
The silica was added in an amount of 0.3% by mass of the phosphoric acid.
Fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
Example 3
Adding 15 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 12 tons of industrial-grade sodium carbonate, stirring to completely dissolve the sodium carbonate, slowly adding wet-process phosphoric acid and 10 tons of solid sodium carbonate under stirring when the temperature of the solution rises to 110 ℃ for reaction, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 3.0, and metering the adding amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.6, adding silicon dioxide, continuing to react for 4 hours, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 420 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
The silica was added in an amount of 0.5% by mass of the phosphoric acid.
Fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
Example 4
Adding 15 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 9 tons of industrial-grade sodium carbonate, stirring to completely dissolve the sodium carbonate, slowly adding wet-process phosphoric acid and 10 tons of solid sodium carbonate under stirring when the temperature of the solution rises to 120 ℃, reacting, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 3.0, and metering the addition amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.6, adding silicon dioxide, continuing to react for 3 hours, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 450 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
The silica was added in an amount of 0.2% by mass of the phosphoric acid.
Fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
Example 5
Adding 15 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 9 tons of soda ash, stirring to completely dissolve the soda ash, slowly adding 85 percent phosphoric acid and 10 tons of solid sodium carbonate under stirring when the temperature of the solution rises to 90 ℃, reacting, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 2.6, and metering the adding amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.4, adding silicon dioxide, continuing to react for 3 hours, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 380 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
In the step, the soda ash is food grade, and the phosphoric acid is thermal phosphoric acid.
In the above reaction, silica was added in an amount of 0.1% by mass of phosphoric acid. The overall reaction process can be represented by the following equation:
6H3PO4+5Na2CO3→4Na2HPO4+2NaH2PO4+5CO2↑+5H2O
NaH2PO4+2Na2HPO4→Na5P3O10+2H2O
fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
The test method is as in example 1, and the results are as follows:
example 6
Adding 15 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 12 tons of soda ash, stirring to completely dissolve the soda ash, slowly adding 85 percent phosphoric acid and 7.5 tons of sodium carbonate under stirring when the temperature of the solution rises to 90 ℃, reacting, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 2.6, and metering the adding amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.4, adding silicon dioxide, continuing to react for 3 hours, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 380 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
In the step, the soda ash is industrial grade and the phosphoric acid is thermal phosphoric acid.
In the above reaction, silica was added in an amount of 0.1% by mass of phosphoric acid. The overall reaction process can be represented by the following equation:
6H3PO4+5Na2CO3→4Na2HPO4+2NaH2PO4+5CO2↑+5H2O
NaH2PO4+2Na2HPO4→Na5P3O10+2H2O
fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
The test method is as in example 1, and the results are as follows:
example 7
Adding 15 tons of water into a neutralization pot, heating to 80 ℃ by using steam, adding 10 tons of food-grade sodium carbonate, stirring to completely dissolve the sodium carbonate, slowly adding wet-process phosphoric acid and 5 tons of solid sodium carbonate under stirring when the temperature of the solution rises to 110 ℃ for reaction, stopping adding acid when the neutralization degree K value of a neutralization solution is adjusted to be 3.0, and metering the adding amount of the phosphoric acid by a metering pump. Controlling the specific gravity of the neutralized slurry to be 1.6, adding silicon dioxide, continuing to react for 4 hours, carrying out fine filtration, then sending into a drying tower, and polymerizing at the reaction temperature of 420 ℃ to generate sodium tripolyphosphate. And (4) after the tail gas passes through an alkaline tower to collect impurity gas, emptying.
The silica was added in an amount of 0.5% by mass of the phosphoric acid.
Other steps were as in example 1, soda ash was food grade and phosphoric acid was wet process phosphoric acid.
Fluoride test method: the fluorine content in the samples was tested according to the method for determining fluoride in the national standard for food safety of GB25566-2010 food additive sodium tripolyphosphate. The food-grade sodium tripolyphosphate requires that the fluoride content is less than or equal to 50 ppm.
Chloride test method: the chlorine content of the samples was determined according to the method specified in the determination of the chloride content of technical sodium tripolyphosphate (including for the food industry) for QB 1036-1991. The detection limit was 30 ppm.
The test method is as in example 1, and the results are as follows:
the above-mentioned embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the present invention, and any modifications, equivalents, improvements and the like made without departing from the technical scope of the present invention as set forth in the claims should be included in the scope of the present invention.
Claims (5)
1. A method for producing sodium tripolyphosphate without chloride and fluoride is characterized in that: the method is realized according to the following steps:
(1) and (3) neutralization reaction: preparing a soda solution with the mass concentration of 30-50%, when the temperature of the solution rises to 90-120 ℃, slowly adding solid sodium carbonate and phosphoric acid while stirring, wherein the phosphoric acid is wet-process phosphoric acid with the mass concentration of 85%, adjusting the K value of the neutralized slurry to be 2.6, controlling the specific gravity of the neutralized slurry to be 1.4-1.6, adding silicon dioxide, the adding amount of the silicon dioxide is 0.1% of the mass of the phosphoric acid, continuously reacting for 3.5 +/-0.5 h to be viscous, filtering to obtain viscous slurry for later use, and converting fluoride and chloride into hydrogen fluoride and hydrogen chloride;
(2) drying and dehydrating: sending the neutralized viscous slurry into a drying tower for atomization and dehydration;
(3) and (3) polymerization generation: carrying out polymerization reaction on the dried and dehydrated raw materials, wherein the polymerization temperature in the polymerization reaction is 380 ℃ to obtain white powdery or fine particle sodium tripolyphosphate;
(4) and (3) carrying out alkaline washing on the tail gas containing hydrogen chloride, hydrogen fluoride and silicon tetrafluoride, and emptying after the tail gas is detected to be qualified.
2. The method of claim 1 for the production of chloride-free, sodium fluoride tripolyphosphate, characterized in that: the particle size of the silicon dioxide is 50-150 mu m.
3. The method of claim 1 for the production of chloride-free, sodium fluoride tripolyphosphate, characterized in that: the temperature of the soda solution is raised to 100 ℃, and then phosphoric acid and solid sodium carbonate are added.
4. The method of claim 1 for the production of chloride-free, sodium fluoride tripolyphosphate, characterized in that: the soda ash is in industrial grade or food grade.
5. The method of claim 1 for the production of chloride-free, sodium fluoride tripolyphosphate, characterized in that: and (2) adding water into a neutralization pot, heating to 80 ℃ by using steam, and adding solid sodium carbonate to completely dissolve the solid sodium carbonate to obtain the required soda solution.
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US4676963A (en) * | 1986-05-09 | 1987-06-30 | Fmc Corporation | Manufacture of sodium tripolyphosphate from wet acid |
CN1539730A (en) * | 2003-10-29 | 2004-10-27 | 张立民 | Novel process for producing sodium tripolyphosphate |
CN101920949A (en) * | 2010-09-19 | 2010-12-22 | 湖北兴发化工集团股份有限公司 | Method for producing nitrate/nitrite-free sodium tripolyphosphate |
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US4676963A (en) * | 1986-05-09 | 1987-06-30 | Fmc Corporation | Manufacture of sodium tripolyphosphate from wet acid |
CN1539730A (en) * | 2003-10-29 | 2004-10-27 | 张立民 | Novel process for producing sodium tripolyphosphate |
CN101920949A (en) * | 2010-09-19 | 2010-12-22 | 湖北兴发化工集团股份有限公司 | Method for producing nitrate/nitrite-free sodium tripolyphosphate |
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