CN1762796A - Preparation method of high-grade sodium hypophosphite - Google Patents
Preparation method of high-grade sodium hypophosphite Download PDFInfo
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- CN1762796A CN1762796A CN 200510015013 CN200510015013A CN1762796A CN 1762796 A CN1762796 A CN 1762796A CN 200510015013 CN200510015013 CN 200510015013 CN 200510015013 A CN200510015013 A CN 200510015013A CN 1762796 A CN1762796 A CN 1762796A
- Authority
- CN
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- Prior art keywords
- solution
- sodium hypophosphite
- nah
- resin
- grade sodium
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Links
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 229910001379 sodium hypophosphite Inorganic materials 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000001556 precipitation Methods 0.000 claims abstract description 23
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 22
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000002500 ions Chemical class 0.000 claims abstract description 14
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 13
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 13
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 10
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 230000006837 decompression Effects 0.000 claims abstract description 3
- 239000003463 adsorbent Substances 0.000 claims abstract 5
- 239000000243 solution Substances 0.000 claims description 84
- 238000000034 method Methods 0.000 claims description 31
- 239000011347 resin Substances 0.000 claims description 22
- 229920005989 resin Polymers 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 9
- 239000012047 saturated solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 229920006395 saturated elastomer Polymers 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 6
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 5
- 230000008929 regeneration Effects 0.000 claims description 5
- 238000011069 regeneration method Methods 0.000 claims description 5
- 239000003729 cation exchange resin Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 230000002829 reductive effect Effects 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims 3
- TVZISJTYELEYPI-UHFFFAOYSA-N hypodiphosphoric acid Chemical compound OP(O)(=O)P(O)(O)=O TVZISJTYELEYPI-UHFFFAOYSA-N 0.000 claims 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 230000007123 defense Effects 0.000 abstract description 4
- 125000002091 cationic group Chemical group 0.000 abstract description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 abstract 2
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- NIAGBSSWEZDNMT-UHFFFAOYSA-M tetraoxidosulfate(.1-) Chemical compound [O]S([O-])(=O)=O NIAGBSSWEZDNMT-UHFFFAOYSA-M 0.000 abstract 1
- 241000370738 Chlorion Species 0.000 description 8
- 238000005406 washing Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000002594 sorbent Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- VUEDNLCYHKSELL-UHFFFAOYSA-N arsonium Chemical compound [AsH4+] VUEDNLCYHKSELL-UHFFFAOYSA-N 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- DTPQZKZONQKKSU-UHFFFAOYSA-N silver azanide silver Chemical compound [NH2-].[Ag].[Ag].[Ag+] DTPQZKZONQKKSU-UHFFFAOYSA-N 0.000 description 2
- 238000004879 turbidimetry Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241001499740 Plantago alpina Species 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention relates to the preparation process of high grade sodium hypophosphite. The preparation process with industrial level sodium hypophosphite as material and active carbon as adsorbent includes silver chloride precipitation to eliminate chlorine ion, barium sulfate precipitation to eliminate sulfate radical ion, sulfide precipitation to eliminate heavy metal ion, addition of small amount of high grade hypophosphorous acid to eliminate micro amount of arsenic, cationic exchanging to prepare high grade sodium hypophosphite solution, decompression enriching, cooling to crystallize, filtering and drying. The product has low contents of hypophosphorous acid, sulfate, chloride, iron and lead. The product may find its wide application in manufacture, electronic industry, national defense industry and other hi-tech fields.
Description
Technical field
The present invention relates to the Preparation of high purity sodium hypophosphite method, it is to be raw material with the technical grade sodium hypophosphite, by removing chlorion, sulfate ion, heavy metal ion, arsonium ion and calcium ion etc. use base exchange method, a kind of method of preparation high grade sodium hypophosphite.
Background technology
Sodium hypophosphite is a kind of comparatively ideal strong reductant, is widely used in high-tech areas such as production, electronic industry, national defense industry, foodstuffs industry, organic synthesis, chemical medical compound probability.Along with going deep into of research and rolling up of its derivative, its Application Areas constantly enlarges, and sodium hypophosphite has become a kind of important inorganic salt product at present.Sodium hypophosphite is widely used mainly as the reductive agent of metal and non-metal material surface electroless plating.In recent years, along with the development of electroless plating, the particularly increase of hard disc of computer demand, the sodium hypophosphite market requirement increases very fast.Sodium hypophosphite demand every year is with 10% to 15% speed increase in the world, and the foreign market transfers from a basic balance that supply falls short of demand to.
The producer that produces sodium hypophosphite in the world mainly contains the STUFF company and the FUKE company of the U.S., German Bi Site Ritz factory and Japanese main road Pharmaceutical Co., Ltd and chemical industry Co., Ltd..China's main manufacturer is chemical plant, Zhangjagang City and Tianjin Sunrise Science and Trade Co., Ltd..Annual about 30,000 tons of China's technical grade sodium hypophosphite output.With regard to sodium hypophosphite, what China's sodium hypophosphite was carried out for a long time is company standard, formulates specialized standard ZBG12018-89 in 2000.The producer or the company of up to the present domestic also not production higher-grade (or claiming electronic-grade) sodium hypophosphite.
Owing to be subjected to the influence of domestic sodium hypophosphite quality, the quality of coating of China's electroless plating is compared with international most advanced level and is also had very big gap, influenced the development of China in high-tech areas such as production, electronic industry, national defense industry, thereby the raising sodium hypophosphite, producing high grade sodium hypophosphite becomes the subject matter that solution is badly in need of in China.At present, also do not have the unified standard of high grade sodium hypophosphite quality product in the world, different high-tech areas is not quite similar to the specification of quality of high grade sodium hypophosphite.The quality product of the high grade sodium hypophosphite of producing should be as the criterion with the needs that satisfy different high-tech areas.
Muriate, vitriol, heavy metal, arsenic and calcium equal size are higher in the technical grade sodium hypophosphite product.Making high grade sodium hypophosphite mainly is to manage to remove these impurity.Removal for these impurity, relevant document carried out preliminary research (Zhang Baogui. Preparation of high purity sodium hypophosphite [J]. inorganic chemicals industry, 2005 03 phases), with the technical grade sodium hypophosphite is raw material, adopt the sedimentary method of silver chloride, barium sulfate and heavy metal sulfide to remove contained chlorion, sulfate radical and heavy metal ion such as iron, lead in the sodium hypophosphite raw material respectively, the relevant technology and the technology of preparation high-purity sodium hypophosphite, and draw optimum process condition and be: Ag
2SO
4Slightly excessive, the optimum temps of removing Cl-is a room temperature, and solution is neutral, adds Ba (OH)
2The about 30min of back churning time.Chloride ion content problem of higher in the high grade sodium hypophosphite product that the weak point of this technology also is not have arsenic removal technology and use the neutralisation preparation.
Summary of the invention
The purpose of this invention is to provide a kind of new Preparation of high purity sodium hypophosphite method, can overcome the shortcoming of prior art.The present invention is to be raw material with the technical grade sodium hypophosphite, by removing chlorion, sulfate ion, and heavy metal ion, arsonium ion and calcium ion etc. use base exchange method, a kind of method of preparation high grade sodium hypophosphite.
Preparation of high purity sodium hypophosphite method of the present invention is to be raw material with the technical grade sodium hypophosphite, adopt the sedimentary method of silver chloride, barium sulfate and heavy metal sulfide to remove contained chlorion, sulfate radical and iron and heavy metal ion in the sodium hypophosphite raw material, it is characterized in that it comprises the steps:
(1) under the room temperature, be that sorbent material uses the silver nitride precipitation method to remove chlorion in the technical grade sodium hypophosphite solution with the gac, at technical grade NaH
2PO
2Add Ag in the solution
2SO
4Saturated solution, milky white precipitate appears, add activated carbon of sorbent again, stirred 10-20 minute, filter;
(2) use barium sulfate precipitate method is removed the sulfate ion in the sodium hypophosphite solution, removes Cl
-After NaH
2PO
2Solution adds saturated Ba (OH)
2Solution fully stirs the back and placed 25-40 minute, makes precipitation fully, filters then;
(3) the use sulphide precipitation is removed the heavy metal ion in the sodium hypophosphite solution, removes Cl
-, SO
4 2-After NaH
2PO
2Add excessive N a slightly in the solution
2The S solid reagent, agitation and filtration, filtrate uses the electronic-grade Hypophosporous Acid, 50 with NaH
2PO
2The hydrogen ion concentration of solution is adjusted to 0.3mol/L, filters and removes micro amount of arsenic impurity.
(4) dilution of the sodium hypophosphite solution after the arsenic removal is 3 times, and the sodium hypophosphite dilute solution is crossed 001 * 7Na type cation exchange resin column with the flow velocity of 1.6-3ml/min, resin column specification φ 30 * 400mm, per 30 minutes sampling analysis H
+Content stops exchange when surpassing index request.
(5) with sodium hypophosphite dilute solution decompression enrichment, cooling, crystallization is filtered, and gets high grade sodium hypophosphite after drying;
(6) regeneration of resin is used pure water drip washing, does not contain H to the exchange column effluent liquid
2PO
2 -, with 4-7ml/min flow velocity drip washing resin, making ion exchange resin conversion is the Na type, is washed till neutrality with pure water with the 10%NaOH of 3 times of volumes, resin is reusable.
Preparation of high purity sodium hypophosphite method of the present invention, it is to be raw material with the technical grade sodium hypophosphite, adopt the sedimentary method of silver chloride, barium sulfate and heavy metal sulfide to remove contained chlorion, sulfate radical and iron and heavy metal ion in the sodium hypophosphite raw material, it is characterized in that it comprises the steps:
(1) under the room temperature, be that sorbent material uses the silver nitride precipitation method to remove chlorion in the technical grade sodium hypophosphite solution, Cl with the gac
-Content be 20-100 μ g/ml, the NaH of 33.33% (weight)
2PO
2Add Ag in the solution
2SO
4Saturated solution, milky white precipitate appears, add activated carbon of sorbent again, stirred 10-20 minute, filter the NaH that obtains
2PO
2The cl content of solution is between the 3-4 μ g/ml; The NaH of every 50ml
2PO
2Add Ag in the solution
2SO
4Saturated solution 1.83-3.50ml; The NaH of every 50ml
2PO
2The add-on of gac is 0.20-0.30g in the solution.
(2) use barium sulfate precipitate method is removed the sulfate ion in the sodium hypophosphite solution, removes Cl
-After NaH
2PO
2Solution adds saturated Ba (OH)
2Solution fully stirs the back and placed 25-40 minute, makes precipitation fully, filters then; Every 50ml NaH
2PO
2Solution needs saturated Ba (OH)
2Solution 3.5-4.5ml;
(3) the use sulphide precipitation is removed the heavy metal ion in the sodium hypophosphite solution, removes Cl
-, SO
4 2-After NaH
2PO
2Add excessive N a slightly in the solution
2The S solid reagent, agitation and filtration, filtrate uses the electronic-grade Hypophosporous Acid, 50 with NaH
2PO
2The hydrogen ion concentration of solution is adjusted to 0.3mol/L, filters and removes micro amount of arsenic impurity; Every 50ml solution adds 0.05g Na
2The S solid.
(4) dilution of the sodium hypophosphite solution after the arsenic removal is 3 times, and the sodium hypophosphite dilute solution is crossed 001 * 7Na type cation exchange resin column with the flow velocity of 1.6-3ml/min, resin column specification φ 30 * 400mm, per 30 minutes sampling analysis H
+Content stops exchange when surpassing index request;
(5) the sodium hypophosphite dilute solution is reduced pressure enrichment, cooling, crystallization is filtered, after drying high grade sodium hypophosphite.The enrichment of reducing pressure of said sodium hypophosphite dilute solution is the enrichment of reducing pressure under 0.07Mpa pressure.
(6) regeneration of resin is used pure water drip washing, does not contain H to the exchange column effluent liquid
2PO
2 -, with 4-7ml/min flow velocity drip washing resin, making ion exchange resin conversion is the Na type, is washed till neutrality with pure water with the 10%NaOH of 3 times of volumes, resin is reusable.
The invention provides a kind of new Preparation of high purity sodium hypophosphite method, can overcome the shortcoming of prior art.The present invention is to be raw material with the technical grade sodium hypophosphite, by removing chlorion, sulfate ion, and heavy metal ion, arsonium ion and calcium ion etc. use base exchange method, a kind of method of preparation high grade sodium hypophosphite.Obtain high grade sodium hypophosphite, wherein NaH
2PO
2H
2O content (%) is 100, H
3PO
3Content (%) is 0.3, vitriol (SO
4) content (%) is 0.0001, muriate (Cl) content (%) is 0.001, and iron (Fe) content (%) is 0.0003, and plumbous (Pb) content (%) is 0.00001, pH (40% solution) 6.5-7.5.The present invention obtains high grade sodium hypophosphite and is widely used in high-tech areas such as production, electronic industry, national defense industry.
Embodiment
Embodiment 1
Get 250g NaH
2PO
2Be dissolved in the 500ml volumetric flask, the sodium hypophosphite solution of preparation 33.33% (weight) uses potentiometric titration to record Cl in the solution
-Content be 60 μ g/ml.
Under the room temperature, preparation Ag
2SO
4Saturated solution: get 3.50g Ag
2SO
4Dissolving, making has solid to exist in the solution, and it is stand-by to get supernatant liquor 250ml.Use atomic absorption spectroscopy to record Ag in the solution
+Content be 0.0463mol/1.Get the NaH of 200ml
2PO
2Solution adds Ag
2SO
4Saturated solution 8.0ml.In this solution, add the sedimentary activated carbon of sorbent 1g of AgCl, stir then, more after filtration, get colourless, clear solution, resulting NaH after about 20 minutes this solution
2PO
2The cl content of solution is between the 3 μ g/ml.
Get 100ml and remove Cl
-After NaH
2PO
2Solution is surveyed SO in the solution with turbidimetry
4 2-Content.Preparation Ba (OH)
2Saturated solution: take by weighing 15.77g Ba (OH)
2Be dissolved in the 500ml volumetric flask, when in the solution a spot of insolubles being arranged, can directly get upper strata liquid and use.With saturated Ba (OH)
2Solution adds this NaH
2PO
2Solution, 100ml NaH
2PO
2Solution needs Ba (OH) approximately
27.5ml.Both under general condition react slower.It is placed half an hour approximately after with magnetic stirrer, makes precipitation fully, filter then, settled solution.Use turbidimetry to record SO in the solution
4 2-Content is almost 0 μ g/ml.Use atomic absorption method to survey and remove Cl
-, SO
4 2-After NaH
2PO
2Ag in the solution
+, pb
2+, Fe
2+Isoionic content is about 0.025,2.0 and 2.5 μ g/ml respectively.
Get the above-mentioned solution of 50ml, add 0.05g Na
2The S solid, agitation and filtration.Use the electronic-grade Hypophosporous Acid, 50 will remove Cl
-, SO
4 2-NaH with heavy metal ion
2PO
2The hydrogen ion concentration of solution is adjusted to 0.3mol/L, filters to remove micro amount of arsenic impurity.
Resin is carried out pre-treatment, and (said pre-treatment is: the saturated aqueous common salt of new resin with 2 times of volumes soaked 24 hours, wash repeatedly with clear water then, till the washing water clarification.NaOH with 4% and 4% HCL and high purity water repetitive scrubbing resin are to remove impurity) with the NaH after the arsenic removal
2PO
23 times of solution dilutions are crossed φ 30 * 400mm 001 * 7Na type cationic exchange coloum, and flow velocity is 2ml/min, removes other cation impurity, the higher-grade NaH that obtains
2PO
2Solution 0.07MPa left and right sides reduction vaporization in the 500ml there-necked flask concentrates, and drying obtains sodium hypophosphite crystal, wherein NaH
2PO
2H
2O content (%) is 100, H
3PO
3Content (%) is 0.3, vitriol (SO
4) content (%) is 0.0001, muriate (Cl) content (%) is 0.001, and iron (Fe) content (%) is 0.0003, and plumbous (Pb) content (%) is 0.00001, pH (40% solution) 6.5-7.5.
(7) regeneration of resin.Use pure water drip washing, do not contain H to the exchange column effluent liquid
2PO
2 -With 4ml/min flow velocity drip washing resin, making ion exchange resin conversion is the Na type, is washed till neutrality with pure water with the 10%NaOH of 3 times of volumes.Resin is reusable.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100150137A CN100351172C (en) | 2005-09-07 | 2005-09-07 | High grade sodium hypophosphite preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100150137A CN100351172C (en) | 2005-09-07 | 2005-09-07 | High grade sodium hypophosphite preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1762796A true CN1762796A (en) | 2006-04-26 |
| CN100351172C CN100351172C (en) | 2007-11-28 |
Family
ID=36747162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100150137A Expired - Fee Related CN100351172C (en) | 2005-09-07 | 2005-09-07 | High grade sodium hypophosphite preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100351172C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101181983B (en) * | 2007-12-12 | 2010-12-22 | 湖北兴发化工集团股份有限公司 | Method for producing hypophosphorous acid |
| CN107478766A (en) * | 2017-07-24 | 2017-12-15 | 湖北省兴发磷化工研究院有限公司 | The method of chloride determination in sodium hypophosphite |
| CN110282610A (en) * | 2019-08-13 | 2019-09-27 | 江苏和纯化学工业有限公司 | The production method of hypophosphorous acid coproduction calcium hypophosphite low cost |
| CN110887888A (en) * | 2019-11-15 | 2020-03-17 | 超威电源集团有限公司 | Method for detecting content of chloride ions in lead-acid storage battery electrolyte |
| CN112047317A (en) * | 2020-08-31 | 2020-12-08 | 江苏康祥实业集团有限公司 | Preparation process of high-grade sodium hypophosphite product |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4379132A (en) * | 1982-08-05 | 1983-04-05 | Fmc Corporation | Process for sodium hypophosphite |
| JPS5992908A (en) * | 1982-11-18 | 1984-05-29 | Nippon Chem Ind Co Ltd:The | Purification of sodium hypophosphite |
| JPH0483709A (en) * | 1990-07-24 | 1992-03-17 | Asahi Chem Ind Co Ltd | Method for purifying sodium hypophosphite |
-
2005
- 2005-09-07 CN CNB2005100150137A patent/CN100351172C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101181983B (en) * | 2007-12-12 | 2010-12-22 | 湖北兴发化工集团股份有限公司 | Method for producing hypophosphorous acid |
| CN107478766A (en) * | 2017-07-24 | 2017-12-15 | 湖北省兴发磷化工研究院有限公司 | The method of chloride determination in sodium hypophosphite |
| CN110282610A (en) * | 2019-08-13 | 2019-09-27 | 江苏和纯化学工业有限公司 | The production method of hypophosphorous acid coproduction calcium hypophosphite low cost |
| CN110887888A (en) * | 2019-11-15 | 2020-03-17 | 超威电源集团有限公司 | Method for detecting content of chloride ions in lead-acid storage battery electrolyte |
| CN112047317A (en) * | 2020-08-31 | 2020-12-08 | 江苏康祥实业集团有限公司 | Preparation process of high-grade sodium hypophosphite product |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100351172C (en) | 2007-11-28 |
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Assignee: Changshu New-tech Chemicals Co., Ltd. Assignor: Nankai University Contract fulfillment period: 2007.12.10 to 2012.12.9 contract change Contract record no.: 2009320001660 Denomination of invention: High grade sodium hypophosphite preparation method Granted publication date: 20071128 License type: exclusive license Record date: 2009.9.8 |
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