CN110342480A - A kind of production method of sodium phosphite - Google Patents
A kind of production method of sodium phosphite Download PDFInfo
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- CN110342480A CN110342480A CN201910773504.XA CN201910773504A CN110342480A CN 110342480 A CN110342480 A CN 110342480A CN 201910773504 A CN201910773504 A CN 201910773504A CN 110342480 A CN110342480 A CN 110342480A
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- Prior art keywords
- sodium
- sodium phosphite
- methanol
- phosphite
- production method
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- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 37
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 76
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000002699 waste material Substances 0.000 claims abstract description 16
- 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 claims abstract description 14
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 14
- 238000002425 crystallisation Methods 0.000 claims abstract description 13
- 230000008025 crystallization Effects 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 23
- 239000012043 crude product Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- KIDXYAWWICJAFK-UHFFFAOYSA-N O.[Na].OC Chemical compound O.[Na].OC KIDXYAWWICJAFK-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000003599 detergent Substances 0.000 abstract description 2
- 230000003827 upregulation Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 244000052616 bacterial pathogen Species 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 3
- 239000000920 calcium hydroxide Substances 0.000 description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005649 metathesis reaction Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- WJEIYVAPNMUNIU-UHFFFAOYSA-N [Na].OC(O)=O Chemical compound [Na].OC(O)=O WJEIYVAPNMUNIU-UHFFFAOYSA-N 0.000 description 1
- GCFSKCZBSOKYLJ-UHFFFAOYSA-N [Na].O[PH2]=O Chemical compound [Na].O[PH2]=O GCFSKCZBSOKYLJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- GRONZTPUWOOUFQ-UHFFFAOYSA-M sodium;methanol;hydroxide Chemical compound [OH-].[Na+].OC GRONZTPUWOOUFQ-UHFFFAOYSA-M 0.000 description 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/163—Phosphorous acid; Salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The present invention provides a kind of production method of sodium phosphite, and it is raw material which, which produces waste residue, after reacting with sodium hydroxide, through filtering, concentration, evaporative crystallization, methanol washing, drying, obtains sodium phosphite product.The production method of sodium phosphite of the invention is using methanol as detergent, it can dissolve and react excessive sodium hydroxide, and insoluble sodium phosphite, the difficulty of industry up-regulation pH is avoided, and this method can recycle excessive sodium hydroxide in reaction, and the methanol solution after washing also can be recycled after distilling, it can effectively save consumption of raw materials, and pollution is not generated, and it is environmentally protective, be conducive to promote efficient utilization of the Sodium hypophosphite production waste residue in production sodium phosphite.
Description
Technical field
The present invention relates to phosphorous chemical industry production technical field, in particular to a kind of production method of sodium phosphite.
Background technique
Sodium phosphite (Sodium phosphite), white crystals type powder, easy to moisture absorption, soluble easily in water, aqueous solution is steady
It is fixed, there is reproducibility.In chemical material field with extensive.
There are mainly three types of existing sodium phosphite production methods: (1) yellow phosphorus is reacted with sodium hydroxide, and primary product is time phosphorus
Sour sodium and sodium phosphite, isolated sodium phosphite product, but two kinds of product separating technologies are complicated；(2) phosphorous acid and hydrogen-oxygen
Change sodium neutralization reaction and, it is easy to operate, but cost of material is higher, industrially have and adjust pH difficulty；(3) the useless of sodium hypophosphite is produced
Slag (mainly containing Arizona bacilli) is reacted with sodium hydroxide or sodium carbonate, and subsequent operation needs to remove excessive sodium hydrate or carbonic acid
Sodium.
It is reacted using the waste residue of production sodium hypophosphite with sodium hydroxide, waste residue can be efficiently used, economize on resources and do not pollute ring
Border, wherein the ingredient for producing the waste residue of sodium hypophosphite is as shown in table 1.
Table 1
In order to make the Arizona bacilli in waste residue be sufficiently converted into sodium phosphite, excessive sodium hydroxide need to be added.Subsequent
In subtractive process, usually using phosphorous acid for adjusting pH, to consume excessive sodium hydroxide.Since the value of acid-base neutralization reaction is presented
It is serious non-linear out, and the reaction mostly occurs in container and circulation line in industry, and the system of resulting in exists simultaneously
Biggish time lag limits the popularization and application of this method so pH value is acknowledged as one of industrial variable most rambunctious.
Summary of the invention
In view of this, the present invention is directed to propose a kind of production method of sodium phosphite, is produced with solving existing sodium phosphite
The problem of pH value regulation difficulty is big in the process, production technology is complicated, high production cost.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of production method of sodium phosphite, comprising the following steps:
1) by the washing of Sodium hypophosphite production waste residue, filtering, filter residue A is obtained；
2) sodium hydrate aqueous solution is added in Xiang Suoshu filter residue A, in nitrogen atmosphere, stirs and heat, then, mistake while hot
Filter, obtains filter residue B and liquor C；
3) by the liquor C concentration, evaporative crystallization, be dried to obtain sodium phosphite crystallization crude product；
4) sodium phosphite is washed with methanol and crystallize crude product, obtain sodium phosphite fine work and sodium hydroxide methanol is molten
Liquid；
5) sodium hydrate methanol solution is distilled, obtains methanol and sodium hydroxide.
Optionally, the water and the Sodium hypophosphite production waste residue of the Sodium hypophosphite production waste residue are washed in the step 1)
Mass ratio > 5: 1.
Optionally, the heating temperature of heating described in the step 2) is 50-150 DEG C, heating time 2-6h.
Optionally, the thickening temperature of the concentration of liquor C described in the step 3) is 80-100 DEG C, the knot of the evaporative crystallization
Brilliant temperature is 40-60 DEG C.
Optionally, concentration >=90% of methanol described in the step 4), and the methanol and the sodium phosphite crystallize
The mass ratio > 1: 10 of crude product.
Compared with the existing technology, the production method of sodium phosphite of the present invention has the advantage that
The present invention is removed the sodium hydroxide in sodium phosphite crude product, is obtained the Asia of high-purity using methanol as detergent
Sodium phosphate product, the methanol solution containing sodium hydroxide obtain methanol and sodium hydroxide, wherein sodium hydroxide energy by distillation
Reaction is enough put into again as raw material, and methanol can also be recycled, so that entire production process does not generate pollutant, and entire
Production process avoids the difficulty of industry up-regulation pH value, can effectively re-use sodium hypophosphite waste residue, in addition, the present invention produces work
Skill is simple, and raw material is cheap to be easy to get, and substantially reduces its production cost, is conducive to industrialization promotion and application of the invention.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 is the production technological process of the sodium phosphite of the embodiment of the present invention 1.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
Below in conjunction with drawings and examples, the present invention will be described in detail.
Embodiment 1
As shown in connection with fig. 1, the production method of the sodium phosphite of the present embodiment, specifically includes the following steps:
1) 10.0g Sodium hypophosphite production waste residue washed with 50mL distilled water, filtered, obtain filter residue A, wherein hypophosphorous acid
Sodium production waste residue is the solid containing Arizona bacilli, calcium hydroxide and a small amount of sodium hypophosphite generated in sodium hypophosphite production course
Residue mainly contains Arizona bacilli and calcium hydroxide in filter residue A；
2) above-mentioned filter residue A, 3.8g sodium hydroxide and 45mL water are placed in reaction vessel, while open stirring, be passed through nitrogen
Air in metathesis reactor is warming up to 100 DEG C, then insulation reaction 4h is filtered while hot, obtains filter residue B and liquor C,
In, filter residue B is mainly calcium hydroxide, and liquor C contains the mixed solution of sodium hydroxide and sodium phosphite, in order to improve filter efficiency
And the recovery efficiency of product, filter residue B can be washed 3 times (10mL/ times), and cleaning solution is merged with liquor C with hot water, be used for
The production of subsequent sodium phosphite；
3) above-mentioned liquor C and cleaning solution are put into evaporating dish, and heat concentration at 100 DEG C, opened in concentration process
Stirring, temperature is down to 65 DEG C and is evaporated crystallization after having crystal precipitation, completely to moisture evaporation, dry phosphorous can be obtained
Sour sodium crystallizes crude product；
4) crude product 3 times (30mL/ times) is crystallized with the above-mentioned sodium phosphite of methanol supersound washing, until can't detect hydroxide
Sodium, filtering, wherein the filter cake being obtained by filtration is dried in vacuo 4h, as the sodium phosphite fine work of high-purity at 65 DEG C, through claiming
Amount, the quality of resulting sodium phosphite fine work are 3.29g, and after testing and calculation, the yield of resulting sodium phosphite fine work is
92.2%, purity 98.4%, filtrate is sodium hydrate methanol solution, i.e., containing the methanol solution of sodium hydroxide；
5) above-mentioned sodium hydrate methanol solution is evaporated under reduced pressure at 35 DEG C, the fraction of collection is methanol, and volume is
82.3mL, and be computed, the rate of recovery 91.4%, and remaining solid is sodium hydroxide, is weighed as 1.36g after dry, and
It is computed, the rate of recovery 88.7%.
Methanol obtained above and sodium hydroxide are recycling in the production of sodium phosphite, specific circulation utilization method
Are as follows:
Water washing 10.0g Sodium hypophosphite production waste residue is distilled with 50mL, after washing, filtering, then, by above-mentioned filtering
Sodium hydroxide, the analytically pure sodium hydroxide of 2.44g and the 45mL water merging reaction vessel of obtained filter cake, 1.36g recycling, simultaneously
Stirring is opened, the air in nitrogen metathesis reactor is led to, is warming up to 100 DEG C, reacts 4h, to after reaction, filter while hot, filter
Cake is washed 2 times with 10mL hot water, merging filtrate and cleaning solution；
Above-mentioned combined filtrate and cleaning solution are put into evaporating dish, and are concentrated in 100 DEG C of heating, there is temperature after crystal precipitation
Degree is down to 65 DEG C of crystallizations, and moisture evaporation obtains sodium phosphite crystallization crude product completely；
Industrial grade benzenemethanol is added in the methanol of recycling to 90ml for washing sodium phosphite crystallization crude product, washs 3 altogether
Secondary (30mL/ times), filtering, wherein the filter cake being obtained by filtration obtains 3.28g sodium phosphite fine work in 65 DEG C of vacuum drying 4h,
Yield is 91.8%, and purity 98.3%, the filtrate being obtained by filtration is evaporated under reduced pressure at 35 DEG C, and obtained fraction is methanol,
Volume is 81.6mL, the rate of recovery 90.7%, and remaining solid is sodium hydroxide, is weighed as 1.30g after dry, is computed
Its, the rate of recovery 84.8%.
It repeats the above steps and recycles methanol and sodium hydroxide, and recycle, to each step under different recycling numbers
The rate of recovery of product calculated, and EDX test is carried out to sodium phosphite fine work, calculates and test result is as shown in table 2.
As shown in Table 2, sodium phosphite is produced using the production method of sodium phosphite of the invention, it can be effectively to methanol and hydrogen
Sodium oxide molybdena is recycled, and gained sodium phosphite yield with higher and purity.
Table 2
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of production method of sodium phosphite, which comprises the following steps:
1) by the washing of Sodium hypophosphite production waste residue, filtering, filter residue A is obtained；
2) sodium hydrate aqueous solution is added in Xiang Suoshu filter residue A, in nitrogen atmosphere, stirs and heat, then, filters while hot,
Obtain filter residue B and liquor C；
3) by the liquor C concentration, evaporative crystallization, be dried to obtain sodium phosphite crystallization crude product；
4) sodium phosphite is washed with methanol and crystallize crude product, obtain sodium phosphite fine work and sodium hydrate methanol solution；
5) sodium hydrate methanol solution is distilled, obtains methanol and sodium hydroxide.
2. the production method of sodium phosphite according to claim 1, which is characterized in that described time of washing in the step 1)
Sodium phosphate produces the water of waste residue and the mass ratio > 5: 1 of the Sodium hypophosphite production waste residue.
3. the production method of sodium phosphite according to claim 1, which is characterized in that heating described in the step 2)
Heating temperature is 50-150 DEG C, heating time 2-6h.
4. the production method of sodium phosphite according to claim 1, which is characterized in that liquor C described in the step 3)
The thickening temperature of concentration is 80-100 DEG C, and the crystallization temperature of the evaporative crystallization is 40-60 DEG C.
5. the production method of sodium phosphite according to claim 1, which is characterized in that methanol described in the step 4)
Concentration >=90%, and the mass ratio > 1: 10 of the methanol and sodium phosphite crystallization crude product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910773504.XA CN110342480A (en) | 2019-08-21 | 2019-08-21 | A kind of production method of sodium phosphite |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910773504.XA CN110342480A (en) | 2019-08-21 | 2019-08-21 | A kind of production method of sodium phosphite |
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Family
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104163410A (en) * | 2014-08-08 | 2014-11-26 | 武汉科技大学 | Method for preparing calcium phosphite from industrial sodium hypophosphite waste residues |
| CN104876201A (en) * | 2014-02-28 | 2015-09-02 | 湖北尧治河化工股份有限公司 | Circulating clean production technology for combined production of sodium hypophosphite, sodium phosphite and calcium hydroxide |
| CN106006676A (en) * | 2016-04-08 | 2016-10-12 | 江苏扬农化工集团有限公司 | Method for recovering sodium hydroxide in H acid alkali fusion process |
-
2019
- 2019-08-21 CN CN201910773504.XA patent/CN110342480A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104876201A (en) * | 2014-02-28 | 2015-09-02 | 湖北尧治河化工股份有限公司 | Circulating clean production technology for combined production of sodium hypophosphite, sodium phosphite and calcium hydroxide |
| CN104163410A (en) * | 2014-08-08 | 2014-11-26 | 武汉科技大学 | Method for preparing calcium phosphite from industrial sodium hypophosphite waste residues |
| CN106006676A (en) * | 2016-04-08 | 2016-10-12 | 江苏扬农化工集团有限公司 | Method for recovering sodium hydroxide in H acid alkali fusion process |
Non-Patent Citations (1)
| Title |
|---|
| 唐世慧等人: "混合水溶液体系中甲醇和氢氧化钠的分离和回收", 《无机盐工业》 * |
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