CN103318861B - Prepare the method for phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate simultaneously - Google Patents
Prepare the method for phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate simultaneously Download PDFInfo
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- CN103318861B CN103318861B CN201310290020.2A CN201310290020A CN103318861B CN 103318861 B CN103318861 B CN 103318861B CN 201310290020 A CN201310290020 A CN 201310290020A CN 103318861 B CN103318861 B CN 103318861B
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Abstract
A kind of method simultaneously preparing phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate.Under nitrogen protection will by sodium phosphorus than being 0.80-0.99, trivalent phosphorus atoms and pentavalent phosphorous atom ratio { P
iII/ P
vbe that the three valent phosphors sodium of 1: 1-2 composition and the mixture of pentavalent phosphorus sodium salt disproportionation and condensation reaction occur by calorifying 200-400 DEG C thus obtains purer phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate.Preparation method provided by the invention avoids phosphine decomposes and oxidation, obtains purer phosphuret-(t)ed hydrogen, prevents environmental pollution.Utilize the existence of phosphuret-(t)ed hydrogen to facilitate the condensation reaction of Trisodium trimetaphosphate simultaneously, obtain the Trisodium trimetaphosphate that purity is higher, avoid the generation of a large amount of long chain macromolecule quantity of material, the technical process of the Trisodium trimetaphosphate shortened, decrease environmental pollution and saved man-hour, reduce production energy consumption, save production cost, make whole Production Flow Chart and the finished product more meet the demand of foodstuffs industry, reach the effect of comprehensive exploitation.
Description
Technical field
The present invention relates to a kind of method producing phosphide, particularly relate to a kind of with the mixture of three valent phosphors sodium salt and pentavalent phosphorus sodium salt for raw material, prepare phosphuret-(t)ed hydrogen (PH simultaneously
3) and Trisodium trimetaphosphate ((NaPO
3)
3) method.
Background technology
Trisodium trimetaphosphate and phosphuret-(t)ed hydrogen are all the very important materials of chemical industry.Trisodium trimetaphosphate is industrially had many uses, especially in starch esterification reaction process.Field of fine chemical all needs highly purified Trisodium trimetaphosphate, requires that its water-insoluble is less than 0.5%, does not contain or contains a small amount of phosphoric acid salt.The preparation of traditional Trisodium trimetaphosphate is via intermediate product by sodium orthophosphate, mainly Sodium Acid Pyrophosphate (acid tetra-sodium) heating (500 DEG C), generate the reactant containing trimetaphosphate composition, this reactant is often mingled with water-fast polyphosphoric acid salt (Maddrell salt).When raw material is by the heating that slowly heats up, can generate a large amount of long chain macromolecule amount sodium polyphosphates, heat this reactant for a long time under more than 500 DEG C of high temperature, this water-fast long-chain sodium polyphosphate can be gradually transformed into Trisodium trimetaphosphate.But the reaction times needed for this method is very long, is generally 24-48 hour, be difficult to be used widely from the viewpoint of economic benefit.Content due to water-insoluble salt reduces the practicality of Trisodium trimetaphosphate, and people did a lot of research, attempts to avoid this composition to produce at the very start or manages the conversion to Trisodium trimetaphosphate of the long chain macromolecule sodium phosphate that accelerates to have generated.For reaching this object, under the high temperature of 500 DEG C to 550 DEG C, rapid heating raw material is the method comparatively commonly used as far as possible, but this technique does not still reach the requirement of foodstuffs industry.
In addition, add the generation that additive can accelerate Trisodium trimetaphosphate in the feed, as: the potassium primary phosphate adding 13%-60% in SODIUM PHOSPHATE, MONOBASIC, the product that clarification is dissolved can be obtained, but the potassium composition containing high density like this is no longer just Trisodium trimetaphosphate, so also inapplicable in many Application Areass.
In addition, many nitride particularly ammonium nitrate, can accelerate generation three metaphosphoric acid.From other method prepared by Trisodium trimetaphosphate, additive can be accelerated Trisodium trimetaphosphate and be formed, and reduces water-insoluble netted sodium polyphosphate salt formation.Volatilizable material is had in these additives, as: ammonium nitrate (US3393974, CN1090255), also the method (US3367737) or heating sodium-chlor and sodium phosphate mixture that add water vapour when preparing Trisodium trimetaphosphate is had, discharge HCl gas (US3347627), object is to keep lower mixture molten state temperature, accelerate the formation reaction of Trisodium trimetaphosphate, as: ammonium salt is exactly (US3393974, the CN1090255) that realize by heating rear generation ammonia NH3 to the booster action that Trisodium trimetaphosphate generates.The shortcoming of these additives is: cannot thoroughly decompose when reaching desirable temperature of reaction, also reduces the purity of finished product accordingly.Such as: the technique that DE1216265 describes, SODIUM PHOSPHATE, MONOBASIC and the mixing of 0.5%-20% ammonium salt, be heated to 300 DEG C to 600 DEG C high temperature with obtained trimetaphosphate, proves have additive to remain in finished product afterwards, which limits product and use field.
However, have incentive very much by the idea adding additive to achieve the goal, people constantly test for this reason.Particularly do not add other compound, and add phosphite phosphorus compound and to make in final product not to be worth exploitation containing the method for other compound.In these techniques, the sodium/phosphorus mol ratio of material solution is greater than 1, and when actually operating, sodium/phosphorus mol ratio is usually between 1.03 to 1.12.Although the long chain macromolecule sodium polyphosphate content in finished product is not high, a large amount of water miscible polyphosphoric acid salts can be produced, especially tripoly phosphate sodium STPP and sodium tetrapolyphosphate.Such as: the technique in DE1266284, the product of these techniques can not meet the requirement that highly purified trimetaphosphate just can reach, and when the phosphite of high density adds Sodium phosphate dibasic mother liquor, can obtain highly purified Trisodium trimetaphosphate.And for example: disclosed in DD78561, the mixture containing high density phosphite generates three metaphosphoric acids of high-quality after being heated to 500 DEG C.Especially mol ratio is the mixed solution of 1: 1 mono phosphoric acid ester sodium and phosphorous acid list sodium, produces this result the most significantly.Because phosphite composition disproportionation when invert point generates phosphuret-(t)ed hydrogen and phosphoric acid salt, the phosphoric acid salt produced by oxidation phosphuret-(t)ed hydrogen in reaction process is by finished absorbent, the sodium phosphorus ratio of such raw material and finished product only has very small change, although have this advantage, this processing disadvantages also clearly: treatment temp is high, phosphite content also must be high as far as possible, the most important thing is, in dismutation, the phosphuret-(t)ed hydrogen of a large amount of high value produced is not used, and whereabouts unknown, this is a potential safety hazard of the method, although become a part for product after inferring the phosphuret-(t)ed hydrogen oxidation discharged, but because the release of phosphuret-(t)ed hydrogen cannot effectively control, the pollution of easy formation product and environment, security can not be guaranteed, in addition, also have to combine and add phosphite and the technique (AT317847) of a small amount of last resultant as initiator, the Trisodium trimetaphosphate added is as substrate, its technique realizes in rotation pipe furnace, this technique phosphite content is not high, but whether the rotation pipe furnace mode of this technique can realize being still problem in rotating table furnace.
Phosphuret-(t)ed hydrogen is the important source material preparing organophosphorus, and also can be mixed for grain depot deinsectization fumigant with carbon dioxide, the high-purity phosphuret-(t)ed hydrogen made after industrial phosphuret-(t)ed hydrogen purifying can be used as processing half guiding element material.It is not high that traditional industry produces phosphuret-(t)ed hydrogen yield, and need consume macroelement phosphorus, purity is also lower, often needs further purification, and easily causes environmental pollution.
Summary of the invention
The object of the invention is the shortcoming overcoming prior art existence, play three valent phosphors sodium salt to greatest extent as the advantage preparing Trisodium trimetaphosphate raw material, provide a kind of mixture by low-temperature heat three valent phosphors sodium salt and pentavalent phosphorus sodium salt under anaerobic to prepare the phosphuret-(t)ed hydrogen of high level and the method for Trisodium trimetaphosphate.
For achieving the above object, the invention provides a kind of method simultaneously preparing phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate, specific as follows:
Mixture three valent phosphors sodium salt and pentavalent phosphorus sodium salt formed, under nitrogen protection by low-temperature heat generation disproportionation and condensation reaction, generates phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate.The sodium phosphorus ratio of the mixture that three valent phosphors sodium salt and pentavalent phosphorus sodium salt are formed is less than 1, and preferably 0.80 ~ 0.99, more preferably 0.85-0.93.
In the present invention, the mixture formed by three valent phosphors sodium salt and pentavalent phosphorus sodium salt, contained trivalent phosphorus atoms and contained pentavalent phosphorous atom ratio { P
iII/ P
vbe 1:1 ~ 2, preferred 1:1.2 ~ 1.4.
In the present invention, the Heating temperature of disproportionation and condensation reaction is 200 DEG C ~ 400 DEG C, preferably 250 DEG C ~ 350 DEG C, as: but be not limited only to 250 DEG C, 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C, 300 DEG C, 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C and 350 DEG C.Three valent phosphors sodium salt disproportionation generate the reaction of phosphuret-(t)ed hydrogen and the condensation reaction equation that meanwhile carries out as follows:
3NaH
2PO
3.H
3PO
3→PH
3+(NaPO
3)
3+3H
2O （1）
3NaH
2PO
4→(NaPO
3)
3+3H
2O （2）
Reaction formula (1) and reaction formula (2) are principal reaction equations of the present invention, and actual generation in the reaction of sodium-metaphosphate and phosphuret-(t)ed hydrogen also has some side reactions, and above two reaction formula can as the standard weighing real reaction and ideal response difference.The yield that phosphorous acid sodium salt disproportionation produces phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate calculates by formula (1) and (1)+(2) respectively.
Three valent phosphors sodium salt as: but be not limited only to phosphorous acid and sodium phosphite.These compounds or be used alone or combinationally use with arbitrary proportion.
Pentavalent phosphorus sodium salt as: but be not limited only to sodium phosphate, Vanadium Pentoxide in FLAKES and phosphoric acid.These compounds or be used alone or combinationally use with arbitrary proportion.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention is according to producing the specified chemical reaction and law of conservation that occur in phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate process, determine sodium phosphorus in raw material than and trivalent phosphorus atoms and pentavalent phosphorous atom ratio, especially sodium phosphorus is a kind of new matching principle than the scheme of < 1, sodium phosphorus ratio in residuum after phosphuret-(t)ed hydrogen in reaction process is discharged completely equals 1, greatly reduce the generation of long chain macromolecule amount chemical substance, thus obtain high-quality Trisodium trimetaphosphate.
Preparation method provided by the invention have employed lower Heating temperature, phosphuret-(t)ed hydrogen is prevented on the one hand to be oxidized and pyrolytic decomposition and dissolving, while obtaining pure phosphuret-(t)ed hydrogen, also facilitate the condensation reaction generating Trisodium trimetaphosphate because of the existence of phosphuret-(t)ed hydrogen, shorten the production cycle of Trisodium trimetaphosphate; Further reduce the generation of long chain macromolecule amount chemical substance on the other hand, thus effectively control reaction process, improve the content of Trisodium trimetaphosphate, obtain more highly purified Trisodium trimetaphosphate, improve yield rate and recovery rate; Adopt lower Heating temperature to reduce products production energy consumption more on the one hand, simplify technical process, saved production cost, improve economic benefit.
Preparation method provided by the invention also adopts the nitrogen formation air flow being a bit larger tham barometric point to enter in reaction flask, both phosphuret-(t)ed hydrogen can have been prevented to be oxidized, be convenient to gather phosphuret-(t)ed hydrogen fast, completely and up hill and dale, prevent phosphuret-(t)ed hydrogen to be dissolved in Trisodium trimetaphosphate, improve the content of Trisodium trimetaphosphate, ensure that the purity of Trisodium trimetaphosphate, phosphuret-(t)ed hydrogen can be prevented again to be dispersed in air simultaneously, contaminate environment, improves production security, adds explained hereafter and is worth.Therefore, make method provided by the invention produce Trisodium trimetaphosphate whole flow process either environmental protection but also economic, or meet the demand of foodstuffs industry.
Embodiment
Below describe technical scheme of the present invention in detail.The embodiment of the present invention is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to the technical scheme of invention or equivalent replacement, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in right of the present invention.
Embodiment 1(A-10V-031/A-10V-032-1)
By phosphorous acid 25g, sodium phosphite prepared by phosphoric acid (85.7%) 26g and sodium hydroxide (96%) 21g and sodium phosphate mixture evaporated under reduced pressure at 70 DEG C, to constant weight, obtains the anhydrous mixing salt 55.8g of theoretical amount, this mixing salt P
iII/ P
vcalculated value is 1.34, it is 0.947 that sodium phosphorus ratio is determined as 0.923(calculated value), the pH value of solution (1%) is 3.34, this mixing salt 30g is placed in the there-necked flask that import and export of nitrogen is housed, with air in nitrogen replacement flask, after half an hour, keep stream of nitrogen gas, pressure is a bit larger tham standard atmospheric pressure, then mixture is warming up to 350 DEG C, material is melting bubbling at this temperature, the phosphuret-(t)ed hydrogen of releasing is brought in the absorption bottle that mercuric chloride solution (2%-3%) is housed by nitrogen, the phosphuret-(t)ed hydrogen of releasing is determined by mercury ion loss amount in weight after drying precipitate in absorption liquid and solution.After bubbling terminates, continue heating 2 hours at the same temperature, stop heating and logical nitrogen, the phosphuret-(t)ed hydrogen weight collected is 0.334 gram, and yield is 25.1%, collect snow-white solid (26.9g in flask, yield 110.5%), solvability inspection display, sample is hardly containing insolubles, solution (1%) pH value is 7.62, ion chromatography Trisodium trimetaphosphate content 98.9%.
Embodiment 2(A-10V-013/A-10V-014-1)
By phosphorous acid 20.1g, sodium phosphite prepared by phosphoric acid (85.7%) 28g and sodium hydroxide (96%) 19.4g and sodium phosphate salt mixture (P
iII/ P
v=1.001) at 70 DEG C evaporated under reduced pressure to constant weight, obtain the anhydrous mixing salt 54.3 grams of theoretical amount, this mixing salt sodium phosphorus than after measured for 0.985(calculated value is 0.950), the pH value of solution (1%) is 3.48, this mixing salt 10g is placed in the there-necked flask that import and export of nitrogen is housed, with air in nitrogen replacement flask, after half an hour, keep stream of nitrogen gas, pressure is a bit larger tham standard atmospheric pressure, then mixture is warming up to 300 DEG C, material is melting bubbling at this temperature, the phosphuret-(t)ed hydrogen of releasing is brought in the absorption bottle that mercuric chloride solution (2-3%) is housed by nitrogen, the phosphuret-(t)ed hydrogen of releasing is determined by mercury ion loss amount in weight after drying precipitate in absorption liquid and solution.After bubbling terminates, continue heating 2 hours at the same temperature, stop heating and logical nitrogen, the phosphuret-(t)ed hydrogen weight collected is 0.1055 gram, yield is 27.5%, collect snow-white solid (9g, yield 108.2%) in flask, solvability inspection display, hardly containing insolubles in sample, the pH value of solution (1%) is 8.04, and ion chromatography display Trisodium trimetaphosphate content 98.9%, its X powder diffraction is analyzed consistent with standard substance.
Embodiment 3(A-11V-064/A-11-065-1)
The sodium phosphite prepared by phosphorous acid 45.1g, phosphoric acid (85.7%) 47.2g and sodium hydroxide (96%) 34.4g and phosphate mixt (P
iII/ P
v=1.33) at 70 DEG C evaporated under reduced pressure to constant weight, obtain the anhydrous mixing salt 104.3 grams of theoretical amount, this mixing salt sodium phosphorus than after measured for 0.896(calculated value is 0.857), the pH value of mixing salt solution (1%) is 2.76, this mixing salt 20g is placed in the there-necked flask that import and export of nitrogen is housed, with air in nitrogen replacement flask, after half an hour, keep stream of nitrogen gas, pressure is a bit larger tham standard atmospheric pressure, then mixture is warming up to 350 DEG C, material is melting bubbling at this temperature, the phosphuret-(t)ed hydrogen of releasing is brought in the absorption bottle that mercuric chloride solution (2-3%) is housed by nitrogen, the phosphuret-(t)ed hydrogen of releasing is determined by mercury ion loss amount in weight after drying precipitate in absorption liquid and solution.After bubbling terminates, continue heating 2 hours at the same temperature, stop heating and logical nitrogen, the phosphuret-(t)ed hydrogen weight collected is 0.345 gram, and yield is 38.5%, collect snow-white solid (17.5g in flask, yield 107.8%), solvability inspection finds that there is a small amount of insolubles, and solution (1%) pH value is 2.79. stratographic analysis Trisodium trimetaphosphate content 84.9%, its X powder diffraction spectrum is composed more known with Trisodium trimetaphosphate standard substance X powder diffraction, and sample contains certain impurity.
Claims (1)
1. prepare the method for phosphuret-(t)ed hydrogen and Trisodium trimetaphosphate for one kind simultaneously; it is characterized in that the sodium phosphorus ratio of described mixture is 0.85 in 250 DEG C ~ 350 DEG C mixtures heating phosphorous acid and sodium phosphate formation or the mixture heating phosphorous acid, sodium phosphite and sodium phosphates formed in 250 DEG C ~ 350 DEG C under nitrogen protection oxygen free condition under nitrogen protection oxygen free condition.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD78561A (en) * | ||||
| US3230039A (en) * | 1962-01-02 | 1966-01-18 | Monsanto Co | Process for manufacturing sodium trimetaphosphate products |
| GB1217011A (en) * | 1968-03-01 | 1970-12-23 | Piesteritz Stickstoff | Glassy sodium polyphosphates |
| AT317847B (en) * | 1970-09-14 | 1974-09-10 | Piesteritz Stickstoff | Process for the preparation of sodium trimetaphosphate |
| CN103253639A (en) * | 2012-12-07 | 2013-08-21 | 江苏先锋生物基技术研究中心有限公司 | Phosphine and sodium trimetaphosphate preparation method |
-
2013
- 2013-07-10 CN CN201310290020.2A patent/CN103318861B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD78561A (en) * | ||||
| US3230039A (en) * | 1962-01-02 | 1966-01-18 | Monsanto Co | Process for manufacturing sodium trimetaphosphate products |
| GB1217011A (en) * | 1968-03-01 | 1970-12-23 | Piesteritz Stickstoff | Glassy sodium polyphosphates |
| AT317847B (en) * | 1970-09-14 | 1974-09-10 | Piesteritz Stickstoff | Process for the preparation of sodium trimetaphosphate |
| CN103253639A (en) * | 2012-12-07 | 2013-08-21 | 江苏先锋生物基技术研究中心有限公司 | Phosphine and sodium trimetaphosphate preparation method |
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Address after: 210048 room D-901/903/905/907, No. 606, Ning six road, Nanjing chemical industry park, Jiangsu, China Patentee after: Nanjing Hongfu high-end phosphine Technology Research Center Co Ltd Address before: 213322, A-2, 18 Tianmu Lake Avenue, Tianmu Lake Industrial Park, Changzhou, Jiangsu, Liyang Patentee before: Changzhou Hongfu High-End Phosphine Technology Co., Ltd. |
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Effective date of registration: 20220602 Address after: 353000 Xingling platform Yanling Road, Jintang Industrial Park, Shaowu, Nanping City, Fujian Province Patentee after: Fujian zhiphosphine Chemical Co.,Ltd. Address before: Room D-901/903/905/907, 606 Ningliu Road, Nanjing Chemical Industrial Park, Jiangsu Province, 210048 Patentee before: NANJING HONGFU HIGH-END PHOSPHINE TECHNOLOGY R&D CENTER |
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