CN104843662A - Preparation method for phosphoric acid sodium salts - Google Patents
Preparation method for phosphoric acid sodium salts Download PDFInfo
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- CN104843662A CN104843662A CN201510177885.7A CN201510177885A CN104843662A CN 104843662 A CN104843662 A CN 104843662A CN 201510177885 A CN201510177885 A CN 201510177885A CN 104843662 A CN104843662 A CN 104843662A
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- phosphoric acid
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- sodium
- sodium phosphate
- phosphate
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- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 87
- 235000019801 trisodium phosphate Nutrition 0.000 claims abstract description 49
- 238000000034 method Methods 0.000 claims abstract description 45
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 39
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 35
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims abstract description 34
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims abstract description 30
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 29
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 20
- 230000007062 hydrolysis Effects 0.000 claims abstract description 18
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 235000011007 phosphoric acid Nutrition 0.000 claims description 46
- 239000012043 crude product Substances 0.000 claims description 35
- 239000012535 impurity Substances 0.000 claims description 32
- 239000003795 chemical substances by application Substances 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 229910001868 water Inorganic materials 0.000 claims description 23
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 18
- 238000000746 purification Methods 0.000 claims description 17
- -1 ortho-phosphoric acid sodium salt Chemical class 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229940001516 sodium nitrate Drugs 0.000 claims description 10
- 235000010344 sodium nitrate Nutrition 0.000 claims description 10
- 239000004317 sodium nitrate Substances 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims description 7
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012452 mother liquor Substances 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical group [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000006227 byproduct Substances 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 6
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 abstract 2
- 229940048086 sodium pyrophosphate Drugs 0.000 abstract 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 abstract 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 abstract 2
- 229910000397 disodium phosphate Inorganic materials 0.000 abstract 1
- 235000019800 disodium phosphate Nutrition 0.000 abstract 1
- 239000006229 carbon black Substances 0.000 description 12
- 238000005406 washing Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
Abstract
The invention discloses a preparation method for phosphoric acid sodium salts, wherein the preparation method comprises the steps: using sodium pyrophosphate as a raw material, carrying out a mixed hydrolysis reaction with wet-process phosphoric acid to obtain sodium orthophosphate, then adding purified wet-process phosphoric acid, adjusting the pH value to obtain disodium phosphate and/or trisodium phosphate, and next carrying out a polymerization reaction to obtain sodium tripolyphosphate. The novel preparation method for the phosphoric acid sodium salts is a new method adopting crude by-products sodium pyrophosphate and sodium hydroxide generated in Caoanning production as the main raw materials and adopting high-temperature and high-pressure hydrolysis process to produce the phosphoric acid sodium salt products. The preparation method is characterized in that the production process is easy to control, the product quality is stable, and the production cost is 35-45% lower than that of a traditional process.
Description
Technical field
The present invention relates to a kind of preparation method of sodium phosphate salt, belong to domain of inorganic chemistry.
Background technology
Sodium salt is a large branch of China's chemical industry, PHOSPHORIC ACID TECH.GRADE disodium, trisodium are one of staple product series of phosphate industry, due to the character that it is special, be widely used in the fields such as modern chemical industry, medicine, food, husbandry, oil, papermaking, washing composition, pottery.
Because sodium phosphate salt end-use is extensive, the huge market demand, main employing thermal phosphoric acid and yellow phosphorus preparing industrial grade 85% acid at present adds soda ash, and neutralisation is produced, and existing tens all manufacturing enterprises of China all adopt this technology to produce this product.This technology production technique due to the main raw material yellow phosphorus thermal phosphoric acid adopted seriously polluted in N-process, energy consumption is surprising, and belong to high energy consumption, high pollution industry, and production cost is also very high.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides a kind of preparation method of Novel phosphoric acid sodium salt.
Object of the present invention carrys out specific implementation by the following technical programs:
A kind of preparation method of sodium phosphate salt, utilize trisodium phosphate for raw material, be obtained by reacting sodium orthophosphate with phosphoric acid by wet process mixed hydrolysis, then add purification of wet process phosphoric acid, obtain Di-Sodium Phosphate and/or tertiary sodium phosphate by adjust ph, then can tripoly phosphate sodium STPP be obtained through polyreaction.
Described trisodium phosphate rather produces produced thick trisodium phosphate from careless amine.
Preferably, the preparation method of above-mentioned sodium phosphate salt, comprises the steps:
1) preparation of ortho-phosphoric acid sodium salt
Crude product trisodium phosphate, water and phosphoric acid by wet process are fully mixed, add removing impurities agent and discoloring agent, be hydrolyzed reaction at temperature is 130-140 DEG C, leaves standstill after reaction, and treat that hydrolysis completely, trisodium phosphate complete reaction generates sodium orthophosphate;
2) preparation of Di-Sodium Phosphate and tertiary sodium phosphate
The ortho-phosphoric acid sodium salt feed liquid filtering and impurity removing that step 1) obtains, add purification of wet process phosphoric acid to be hydrolyzed further, when regulating pH to be 7.5, complete reaction generates Di-Sodium Phosphate, and when regulating pH to be 13, complete reaction generates tertiary sodium phosphate, according to demand, regulate pH, then be cooled to and be less than 18 DEG C, obtain corresponding Na2PO412H2O and/or Na3PO412H2O crystal;
3) preparation of tripoly phosphate sodium STPP
By step 2) Di-Sodium Phosphate prepared adds neutralizing well, mix with phosphoric acid by wet process after heating for dissolving, control pH is 6.5, at 70-80 DEG C, adds SODIUMNITRATE, neutralization reaction completely after, feed liquid is placed in polymerization furnace and carries out polyreaction, obtain tripolyphosphate sodium salt.
Preferably, in described step 1), the weight ratio of crude product trisodium phosphate, water and phosphoric acid by wet process is 1:2:0.1.
Preferably, in described step 1), the pressure of hydrolysis reaction is 0.2MPa, and hydrolysis temperature is by automatic steam control, and optimum hydrolysis temperature is 135 DEG C.
Preferably, in described step 1), described removing impurities agent is Sodium Sulphide, and every 1000 kilograms of crude product trisodium phosphates add removing impurities agent 5-7 kilogram, preferably 6 kilograms; Described discoloring agent is activated carbon, and every 1000 kilograms of crude product trisodium phosphates add discoloring agent 5-7 kilogram, preferably 6 kilograms.
Preferably, in described step 1), before reaction, first water washing is added to crude product trisodium phosphate and be less than 1% to NaCI content.
Preferably, described step 2) in, after step 1) gained feed liquid filtering and impurity removing, through supernatant, after naturally cooling to 30-40 DEG C, then be hydrolyzed further.Owing to containing the impurity such as carbon black in crude product trisodium phosphate, the liquid after dissolving filters, and removes the impurity such as carbon black.Carbon black after filtration is with after a little clear water washing, and filter residue is taken out as by-product.
Described step 2) in, after hydrolysis crystallize out, by centrifugation, mother liquor is used as hydrolysis reaction water circulation use.
Preferably, described step 2) in, the amount adding purification of wet process phosphoric acid is: every 1000 kilograms of crude product trisodium phosphates add purification of wet process phosphoric acid 185-200 kilogram, preferably 190 kilograms.
Preferably, in described step 3), Di-Sodium Phosphate: the weight ratio of SODIUMNITRATE is 1.63.
Preferably, in described step 3), polymerization temperature is 380-420
oc, polymerization time is 2 hours.
Beneficial effect:
The preparation method of novel sodium phosphate salt provided by the invention is that rather to produce produced by-product crude product trisodium phosphate and sodium hydroxide with careless amine be that main raw material adopts high temperature, high-pressure hydrolysis process to produce the novel method of sodium phosphate salt product.The feature of this technology is that production technique is easy to control, and constant product quality, production cost is lower than traditional technology 35-45%.Key make use of the peaceful by-product trisodium phosphate of careless amine, belong to originally and stack in useless waste, not only environment is affected, and cause certain environment pressure and production cost pressure to upstream firm, and pass through the utilization of this technology, original waste product is turned waste into wealth, solve the environmental protection trouble and worry of enterprise, and add an extra income to enterprise, thus reduce further the production cost of enterprise, add profit; Also the scope that Chemical Manufacture recycling economy country encourages is belonged to.The success of this new technology, to the environment protection of upstream and downstream firms, production cost, contribution maximum beyond doubt, also for national environment protection, making full use of of resource have made achievement.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Crude product trisodium phosphate in following embodiment rather produces produced thick trisodium phosphate from careless amine.
embodiment 1:
A preparation method for sodium phosphate salt,
1) preparation of ortho-phosphoric acid sodium salt
First water washing is added to crude product trisodium phosphate and be less than 1% to NaCI content, crude product trisodium phosphate, water and phosphoric acid by wet process are fully mixed, add removing impurities agent and discoloring agent, to be hydrolyzed at temperature is 135 DEG C reaction by automatic steam control, the pressure of hydrolysis reaction is 0.2MPa, leave standstill, treat that hydrolysis completely, trisodium phosphate complete reaction generates sodium orthophosphate;
2) preparation of Di-Sodium Phosphate and tertiary sodium phosphate
To after step 1) gained feed liquid filtering and impurity removing (due in crude product trisodium phosphate containing the impurity such as carbon black, liquid after dissolving filters, and removes the impurity such as carbon black, and the carbon black after filtration is with after a little clear water washing, filter residue is taken out as by-product), through supernatant, after naturally cooling to 30-40 DEG C, add purification of wet process phosphoric acid and be hydrolyzed further, when regulating pH to be 7.5, complete reaction generates Di-Sodium Phosphate, then is cooled to and is less than 18 DEG C, obtains corresponding Na2PO412H2O crystal;
3) preparation of tripoly phosphate sodium STPP
By step 2) Di-Sodium Phosphate prepared adds neutralizing well, mix with phosphoric acid by wet process after heating for dissolving, control pH is 6.5, at 70-80 DEG C, adds SODIUMNITRATE, neutralization reaction completely after, feed liquid is placed in polymerization furnace and carries out polyreaction, obtain tripolyphosphate sodium salt.
In described step 1), the weight ratio of crude product trisodium phosphate, water and phosphoric acid by wet process is 1:2:0.1.
Preferably, in described step 1), described removing impurities agent is Sodium Sulphide, and every 1000 kilograms of crude product trisodium phosphates add removing impurities agent 6 kilograms; Described discoloring agent is activated carbon, and every 1000 kilograms of crude product trisodium phosphates add discoloring agent 6 kilograms.
Described step 2) in, after hydrolysis crystallize out, by centrifugation, mother liquor is used as hydrolysis reaction water circulation use.
Described step 2) in, the amount adding purification of wet process phosphoric acid is: every 1000 kilograms of crude product trisodium phosphates add purification of wet process phosphoric acid 190 kilograms.
In described step 3), Di-Sodium Phosphate: the weight ratio of SODIUMNITRATE is 1.63.
In described step 3), polymerization temperature is 400
oc, polymerization time is 2 hours
embodiment 2:
A preparation method for sodium phosphate salt,
1) preparation of ortho-phosphoric acid sodium salt
First water washing is added to crude product trisodium phosphate and be less than 1% to NaCI content, crude product trisodium phosphate, water and phosphoric acid by wet process are fully mixed, add removing impurities agent and discoloring agent, be hydrolyzed at being 130 DEG C by automatic steam control temperature reaction, the pressure of hydrolysis reaction is 0.2MPa, leave standstill after reaction, treat that hydrolysis completely, trisodium phosphate complete reaction generates sodium orthophosphate;
2) preparation of Di-Sodium Phosphate and tertiary sodium phosphate
The ortho-phosphoric acid sodium salt feed liquid filtering and impurity removing that step 1) obtains, add purification of wet process phosphoric acid to be hydrolyzed further, when regulating pH to be 7.5, complete reaction generates Di-Sodium Phosphate, be cooled to again and be less than 18 DEG C, obtain corresponding Na2PO412H2O and/or Na3PO412H2O crystal;
3) preparation of tripoly phosphate sodium STPP
By step 2) Di-Sodium Phosphate prepared adds neutralizing well, mix with phosphoric acid by wet process after heating for dissolving, control pH is 6.5, at 70-80 DEG C, adds SODIUMNITRATE, neutralization reaction completely after, feed liquid is placed in polymerization furnace and carries out polyreaction, obtain tripolyphosphate sodium salt.
In described step 1), the weight ratio of crude product trisodium phosphate, water and phosphoric acid by wet process is 1:2:0.1.
In described step 1), described removing impurities agent is Sodium Sulphide, and every 1000 kilograms of crude product trisodium phosphates add removing impurities agent 5 kilograms; Described discoloring agent is activated carbon, and every 1000 kilograms of crude product trisodium phosphates add discoloring agent 7 kilograms.
Described step 2) in, after step 1) gained feed liquid filtering and impurity removing, through supernatant, after naturally cooling to 30-40 DEG C, then be hydrolyzed further.Owing to containing the impurity such as carbon black in crude product trisodium phosphate, the liquid after dissolving filters, and removes the impurity such as carbon black.Carbon black after filtration is with after a little clear water washing, and filter residue is taken out as by-product.
Described step 2) in, after hydrolysis crystallize out, by centrifugation, mother liquor is used as hydrolysis reaction water circulation use.
Described step 2) in, the amount adding purification of wet process phosphoric acid is: every 1000 kilograms of crude product trisodium phosphates add purification of wet process phosphoric acid 185 kilograms.
In described step 3), Di-Sodium Phosphate: the weight ratio of SODIUMNITRATE is 1.63.
In described step 3), polymerization temperature is 380
oc, polymerization time is 2 hours
embodiment 3:
A preparation method for sodium phosphate salt,
1) preparation of ortho-phosphoric acid sodium salt
First water washing is added to crude product trisodium phosphate and be less than 1% to NaCI content, crude product trisodium phosphate, water and phosphoric acid by wet process are fully mixed, add removing impurities agent and discoloring agent, to be hydrolyzed at temperature is 140 DEG C reaction by automatic steam control, the pressure of hydrolysis reaction is 0.2MPa, leave standstill after reaction, treat that hydrolysis completely, trisodium phosphate complete reaction generates sodium orthophosphate;
2) preparation of Di-Sodium Phosphate and tertiary sodium phosphate
The ortho-phosphoric acid sodium salt feed liquid filtering and impurity removing that step 1) obtains, add purification of wet process phosphoric acid to be hydrolyzed further, when regulating pH to be 7.5, complete reaction generates Di-Sodium Phosphate, and when regulating pH to be 13, complete reaction generates tertiary sodium phosphate, according to demand, regulate pH, then be cooled to and be less than 18 DEG C, obtain corresponding Na2PO412H2O and/or Na3PO412H2O crystal;
3) preparation of tripoly phosphate sodium STPP
By step 2) Di-Sodium Phosphate prepared adds neutralizing well, mix with phosphoric acid by wet process after heating for dissolving, control pH is 6.5, at 70-80 DEG C, adds SODIUMNITRATE, neutralization reaction completely after, feed liquid is placed in polymerization furnace and carries out polyreaction, obtain tripolyphosphate sodium salt.
In described step 1), the weight ratio of crude product trisodium phosphate, water and phosphoric acid by wet process is 1:2:0.1.
In described step 1), described removing impurities agent is Sodium Sulphide, and every 1000 kilograms of crude product trisodium phosphates add removing impurities agent 7 kilograms; Described discoloring agent is activated carbon, and every 1000 kilograms of crude product trisodium phosphates add discoloring agent 5 kilograms.
Described step 2) in, after step 1) gained feed liquid filtering and impurity removing, through supernatant, after naturally cooling to 30-40 DEG C, then be hydrolyzed further.Owing to containing the impurity such as carbon black in crude product trisodium phosphate, the liquid after dissolving filters, and removes the impurity such as carbon black.Carbon black after filtration is with after a little clear water washing, and filter residue is taken out as by-product.
Described step 2) in, after hydrolysis crystallize out, by centrifugation, mother liquor is used as hydrolysis reaction water circulation use.
Described step 2) in, described step 2) in, the amount adding purification of wet process phosphoric acid is: every 1000 kilograms of crude product trisodium phosphates add purification of wet process phosphoric acid 200 kilograms.
In described step 3), Di-Sodium Phosphate: the weight ratio of SODIUMNITRATE is 1.63.
In described step 3), polymerization temperature is 420
oc, polymerization time is 2 hours
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a sodium phosphate salt, it is characterized in that: utilize trisodium phosphate for raw material, be obtained by reacting sodium orthophosphate with phosphoric acid by wet process mixed hydrolysis, then add purification of wet process phosphoric acid, obtain Di-Sodium Phosphate and/or tertiary sodium phosphate by adjust ph, then can tripoly phosphate sodium STPP be obtained through polyreaction.
2. the preparation method of sodium phosphate salt according to claim 1, is characterized in that: described trisodium phosphate rather produces produced thick trisodium phosphate from careless amine.
3. the preparation method of sodium phosphate salt according to claim 1 and 2, is characterized in that: comprise the steps:
1) preparation of ortho-phosphoric acid sodium salt
Crude product trisodium phosphate, water and phosphoric acid by wet process are fully mixed, add removing impurities agent and discoloring agent, be hydrolyzed reaction at temperature is 130-140 DEG C, leaves standstill after reaction, and treat that hydrolysis completely, trisodium phosphate complete reaction generates sodium orthophosphate;
2) preparation of Di-Sodium Phosphate and tertiary sodium phosphate
The ortho-phosphoric acid sodium salt feed liquid filtering and impurity removing that step 1) obtains, add purification of wet process phosphoric acid to be hydrolyzed further, when regulating pH to be 7.5, complete reaction generates Di-Sodium Phosphate, and when regulating pH to be 13, complete reaction generates tertiary sodium phosphate, according to demand, regulate pH, then be cooled to and be less than 18 DEG C, obtain corresponding Na
2pO
412H
2o and/or Na
3pO
412H
2o crystal;
3) preparation of tripoly phosphate sodium STPP
By step 2) Di-Sodium Phosphate prepared adds neutralizing well, mix with phosphoric acid by wet process after heating for dissolving, control pH is 6.5, at 70-80 DEG C, adds SODIUMNITRATE, neutralization reaction completely after, feed liquid is placed in polymerization furnace and carries out polyreaction, obtain tripolyphosphate sodium salt.
4. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: in described step 1), and the weight ratio of crude product trisodium phosphate, water and phosphoric acid by wet process is 1:2:0.1;
Preferably, the pressure of hydrolysis reaction is 0.2MPa, and hydrolysis temperature is by automatic steam control, and optimum hydrolysis temperature is 135 DEG C.
5. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: in described step 1), and described removing impurities agent is Sodium Sulphide, and every 1000 kilograms of crude product trisodium phosphates add removing impurities agent 5-7 kilogram, preferably 6 kilograms; Described discoloring agent is activated carbon, and every 1000 kilograms of crude product trisodium phosphates add discoloring agent 5-7 kilogram, preferably 6 kilograms.
6. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: described step 2) in, after step 1) gained feed liquid filtering and impurity removing, through supernatant, after naturally cooling to 30-40 DEG C, then be hydrolyzed further.
7. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: described step 2) in, after hydrolysis crystallize out, by centrifugation, mother liquor is used as hydrolysis reaction water circulation use.
8. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: described step 2) in, the amount adding purification of wet process phosphoric acid is: every 1000 kilograms of crude product trisodium phosphates add purification of wet process phosphoric acid 185-200 kilogram, preferably 190 kilograms.
9. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: in described step 3), Di-Sodium Phosphate: the weight ratio of SODIUMNITRATE is 1.63.
10. the preparation method of sodium phosphate salt according to claim 3, is characterized in that: in described step 3), and polymerization temperature is 380-420
oc, polymerization time is 2 hours.
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| CN106335889A (en) * | 2016-08-18 | 2017-01-18 | 宜宾天原集团股份有限公司 | Method for producing sodium tripolyphosphate by utilization of crude sodium pyrophosphate |
| CN108178138A (en) * | 2016-12-08 | 2018-06-19 | 江苏优士化学有限公司 | A kind of production technology of new trimerization sodium phosphate |
| 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 |
| CN109455685A (en) * | 2018-12-28 | 2019-03-12 | 湖北泰盛化工有限公司 | A kind of method that the purification of crude product sodium pyrophosphate produces sodium dihydrogen phosphate and sodium chloride |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106335889A (en) * | 2016-08-18 | 2017-01-18 | 宜宾天原集团股份有限公司 | Method for producing sodium tripolyphosphate by utilization of crude sodium pyrophosphate |
| CN106335889B (en) * | 2016-08-18 | 2018-09-25 | 宜宾天原集团股份有限公司 | The method for producing sodium tripolyphosphate using thick sodium pyrophosphate |
| CN108178138A (en) * | 2016-12-08 | 2018-06-19 | 江苏优士化学有限公司 | A kind of production technology of new trimerization sodium phosphate |
| CN108178138B (en) * | 2016-12-08 | 2020-01-07 | 江苏优士化学有限公司 | Production process of novel sodium tripolyphosphate |
| 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 |
| CN109455685A (en) * | 2018-12-28 | 2019-03-12 | 湖北泰盛化工有限公司 | A kind of method that the purification of crude product sodium pyrophosphate produces sodium dihydrogen phosphate and sodium chloride |
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| CN104843662B (en) | 2018-02-23 |
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