CN103787293A - Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process - Google Patents
Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process Download PDFInfo
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- CN103787293A CN103787293A CN201410035054.1A CN201410035054A CN103787293A CN 103787293 A CN103787293 A CN 103787293A CN 201410035054 A CN201410035054 A CN 201410035054A CN 103787293 A CN103787293 A CN 103787293A
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- monobasic
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Abstract
The invention discloses a method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process. The method comprises the steps of carrying out reaction on carbamide and the phosphoric acid by the wet process to obtain intermediate, and then carrying out a reaction on the intermediate and sodium hydroxide to obtain the sodium dihydrogen phosphate product. The method is short in process route, low in energy consumption, stable in product quality, low in production cost, convenient to operate and safe in production; the by-product slurry can be completely recycled; the whole production process is environment-friendly, clean and free from pollution as well as emission of waste gas, waste water and waste residue; therefore, the method responses to the policy of energy conservation and emission reduction as well as clean production, and solves the problems of complicated technology, unstable product quality, high energy consumption, environmental pollution and the like in the prior art; the obtained sodium dihydrogen phosphate product has the purity of more than or equal to 98%.
Description
Technical field
The present invention relates to a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process, belong to chemical technology field.
Background technology
SODIUM PHOSPHATE, MONOBASIC is of many uses, can be as the raw material of manufacturing Sodium hexametaphosphate 99 and trisodium phosphate; Also can be used for process hides, process feedwater; As quality improver and baking powder processed, in foodstuffs industry, fermentation industry, make buffer reagent and saleratus raw material; Also be used as fodder additives, washing composition and dye auxiliary agent etc.; In foodstuffs industry, fermentation industry, also can be used as buffer reagent, as the raw material of saleratus, make bread, sizing and the ripening agent of sauce, powder acidic flavoring agent, is cooked the quality improver of evaporated milk; Also can do stablizer, the cakingagent of the milk-product such as cheese, meat, fish product, bake the buffer reagent of powder, pickle with mixing salt etc.But current SODIUM PHOSPHATE, MONOBASIC suitability for industrialized production, because Wet Processes of Phosphoric Acid is still immature, cannot realize suitability for industrialized production, causes production method limited, be substantially all to adopt thermal phosphoric acid or Wet Phosphoric Acid Market to react and make with potassium hydroxide or sodium carbonate.The main production method of SODIUM PHOSPHATE, MONOBASIC has two kinds now, and one is SODIUM PHOSPHATE, MONOBASIC neutralisation, and another kind is alkali neutralisation.SODIUM PHOSPHATE, MONOBASIC neutralisation is that SODIUM PHOSPHATE, MONOBASIC is dissolved, and adds the phosphoric acid of metering to neutralize, through condensing crystal, the dry product that to obtain; Alkali neutralisation is with phosphoric acid and sodium carbonate or sodium hydroxide neutralization, pH value is adjusted to 4.4-4.6 and filters, and concentrating filter liquor crystallizing and drying obtains product.In above two kinds of methods, phosphoric acid used is Wet Phosphoric Acid Market or thermal phosphoric acid, and two kinds of methods all have concentrating unit in addition, therefore production cost is high.The shortcoming of thermal phosphoric acid method is that in production process, energy consumption is high, pollutes greatly, and along with energy shortage, environmental pollution is more and more serious, and thermal phosphoric acid is produced the restriction that is subject to national policy; The deficiency of wet phosphoric acid purifying method is that operational path is long, and plant construction investment is large, causes production cost high, adopts thermal phosphoric acid or Wet Phosphoric Acid Market production SODIUM PHOSPHATE, MONOBASIC all exists a lot of unfavorable factors.In sum, the biphosphate production method of sodium ubiquity of prior art that energy consumption is high, by product is difficult to processing, unstable product quality and economic benefit bad, be unfavorable for the problems such as environmental protection.
The method of a kind of calcium formiate as disclosed in CN101475463A and peroxophosphoric acid reaction co-producing high-purity formic acid and SODIUM PHOSPHATE, MONOBASIC: carbon monoxide enters reaction three towers; Calcium hydroxide enters reaction one tower, carry out countercurrent reaction with the carbon monoxide that carrys out autoreaction two towers, reaction solution overflow is to reacting two towers, with the carbon monoxide gas countercurrent reaction that carrys out autoreaction three towers, reaction solution enters reaction three towers, carry out countercurrent reaction with carbon monoxide, reaction solution enters discharge tank by reacting three tower overflows, makes calcium formiate and prepares liquid; This calcium formiate is prepared liquid, enters reactor, drips formic acid, passes into hydrogen sulfide, separates filter residue through filter I, and filtrate enters continuous crystallizer, and crystal solution enters strainer II, and the calcium formiate drying device after filtration is made finished product calcium formiate; Peroxophosphoric acid, formic acid and calcium formiate are input into into horizontal double-screw reactor, generate formic acid and monocalcium phosphate, enter the underpressure distillation of formic acid distillation still, and monocalcium phosphate is transported to monocalcium phosphate metering receiving tank, and formic acid enters formic acid receiving tank.The deficiency of this scheme is technique complex circuit, and energy consumption is high, and the SODIUM PHOSPHATE, MONOBASIC product purity and the quality that generate are unstable.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process, solve in existing SODIUM PHOSPHATE, MONOBASIC production technology technique circuit longer, unstable product quality, energy consumption is high, and by product is difficult and be unfavorable for the problem of environmental protection.
Preparing a method for SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process, is to utilize carboxamide and wet-process phosphoric acid reaction to obtain intermediate, then this intermediate is reacted to preparation SODIUM PHOSPHATE, MONOBASIC product with sodium hydroxide.
Of the present inventionly comprise the following steps by the method that phosphoric acid by wet process is prepared SODIUM PHOSPHATE, MONOBASIC:
(1) removal of impurities of phosphoric acid by wet process:
Adopt method centrifugal or press filtration to remove the solid impurity containing in phosphoric acid by wet process, obtain phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 40 ℃-90 ℃, under agitation condition, add carboxamide and phosphoric acid to carry out building-up reactions, the add-on of carboxamide is (0.9-1.05) by it with the mol ratio of phosphoric acid: 1 is definite, and the reaction times is 40min-120min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove and be cooled to temperature≤40 ℃, centrifugation, retains filter cake, and filter cake is intermediate, puts into intermediate warehouse, for subsequent use;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add the sodium hydroxide hybrid reaction of metering, the mol ratio of described intermediate and sodium hydroxide is (1-1.2): 1, and that controls sodium hydroxide adds speed to regulate the temperature of synthesizing in groove within the scope of 40 ℃-90 ℃, stirring reaction 20min-100min; After reaction finishes, SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature≤40 ℃, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide, reclaims carboxamide wherein, returns to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, dry rear packing.
Intermediate in described step (2) is CO (NH
2)
2h
3pO
4.
In described step (1), phosphoric acid by wet process concentration is 15%-75%.
After carboxamide being formulated as to carbon amide solution in described step (2), carry out building-up reactions with phosphoric acid again.
In described step (3), centrifugation gained filtrate is the intermediate slip that contains impurity, delivers to composite fertilizer production line production composite fertilizer.
In described step (4), dissolution of sodium hydroxide is obtained reacting with intermediate solid after sodium hydroxide solution.
In described step (4), dissolution of sodium hydroxide being obtained to dissolve with intermediate the solution obtaining after sodium hydroxide solution reacts.
In described step (4), intermediate being dissolved to the solution obtaining reacts with sodium hydrate solid.
Described step (4) Raw sodium hydroxide is replaceable is sodium carbonate, and the mol ratio of described intermediate and sodium carbonate is (2.0～2.05): 1.
Carboxamide of the present invention preferentially selects market to sell the carboxamide of fertilizer grade, and consumption is pressed carboxamide and phosphoric acid by wet process mol ratio (0.9-1.05): 1 determines.Carboxamide is reacted again to SODIUM PHOSPHATE, MONOBASIC product purity >=98% obtaining with sodium hydroxide with the intermediate obtaining after wet-process phosphoric acid reaction.The SODIUM PHOSPHATE, MONOBASIC product purity of products obtained therefrom of the present invention and traditional thermal phosphoric acid neutralisation is close, and complicated process of preparation degree and cost drop into well below traditional thermal phosphoric acid neutralisation.Applicant is through the discovery that studies for a long period of time, and the intermediate that carboxamide and phosphoric acid generate, can generate highly purified SODIUM PHOSPHATE, MONOBASIC product with sodium hydroxide.
Carboxamide of the present invention is that (molecular formula is CO (NH to urea
2)
2):
Carboxamide is colourless or white needles or bar-shaped xln, and water-soluble, alcohol, is insoluble in ether, chloroform, is weakly alkaline; Industrial or agriculture product are slightly blush solid particulate of white, have pungent smell.The nitrogen content of carboxamide is about 46.67%, is that in solid nitrogenous fertilizer, nitrogen content is the highest.Carboxamide has hydrolytic action, can generate salt with acid effect.Because contain this material in people and mammiferous urine, have another name called urea or urea.Carboxamide has amide structure, therefore have the general chemical property of acid amides, owing to there being two amino to be directly connected with carbonyl, they influence each other, and makes carboxamide different from general acid amides, and shows some special propertys.In carboxamide molecule, the not share electron pair on two nitrogen-atoms all with carbonyl π-electron generation conjugative effect, therefore compared with acid amides, cloud density on nitrogen-atoms reduces less, stronger with the binding ability of proton, so the alkalescence of carboxamide is slightly stronger than acid amides, can produce salt with strong acid.Because the salt generating is crystal, be slightly soluble in water, be insoluble to acid, utilize this character just carboxamide can be separated.Under the effect of acid, alkali or urease, easily there is hydrolysis reaction in carboxamide, generates ammonia and carbonic acid gas, therefore carboxamide can be used as high-efficiency nitrogen fertilizer.Phosphorus and nitrogen belong to same main group, and character is quite approaching.In the time that carboxamide adopts urea, intermediate of the present invention is Ureaphil CO (NH
2)
2h
3pO
4.As can be seen here, carboxamide and wet-process phosphoric acid reaction, the intermediate obtaining has certain chemical property, can generate the SODIUM PHOSPHATE, MONOBASIC product that purity is higher with sodium hydroxide.In addition, sodium hydroxide is also replaceable is sodium carbonate, also can obtain the SODIUM PHOSPHATE, MONOBASIC that purity is higher.
In the present invention, in the time of phosphatase reaction after carboxamide and removal of impurities, can be first by carboxamide with after water dissolution, be prepared into carbon amide solution again with phosphatase reaction, also carboxamide solid directly can be reacted with phosphoric acid; In the time that intermediate reacts with sodium hydroxide, can be that carbon amide solution reacts with sodium hydrate solid, or carbon amide solution react with sodium hydroxide solution, can be also sodium hydroxide solution and carboxamide solid reaction.
The chemical equation relating in the present invention is as follows:
Phosphoric acid by wet process reacts with carboxamide and obtains highly purified intermediate:
H
3PO
4+CO(NH
2)
2=CO(NH
2)
2·H
3PO
4
React again preparation SODIUM PHOSPHATE, MONOBASIC with intermediate with sodium carbonate/sodium hydroxide, in reacted slip, contain carboxamide:
CO(NH
2)
2·H
3PO
4+NaOH=NaH
2PO
4+CO(NH
2)
2+H
2O
2CO(NH
2)
2·H
3PO
4+Na
2CO
3=2NaH
2PO
4+2CO(NH
2)
2+H
2O+CO
2
In the present invention, described intermediate is Ureaphil (Ureaphosphate, UP), is for No. CAS 4861-19-2, and molecular formula is CH
7n
2o
5p, can be expressed as CO (NH
2)
2h
3pO
4:
Ureaphil is a kind of fine chemical product that is widely used in the fields such as livestock industry, industry, agricultural, its solid is white crystals or crystalline powder, and soluble in water and alcohol is insoluble to ethers, toluene and tetracol phenixin, it is acid that the aqueous solution is, and starts to decompose to emit carbonic acid gas and ammonia when melting.The clear solution that Ureaphil of the prior art normally obtains after Hybrid Heating stirs certain hour with phosphoric acid and urea, then be positioned over crystallization in cooling tank, the dry Ureaphil product that obtains after filtering.Phosphoric acid can adopt thermal phosphoric acid or phosphoric acid by wet process.The strong phosphoric acid of the common employing 40%～54% of phosphoric acid by wet process or 25% dilute phosphoric acid are that raw material is prepared Ureaphil; Also can add in process of production some additives, cause the purity of commercially available Ureaphil product not high enough; Such as in the time adopting 25% dilute phosphoric acid, can add defluorinating agent sodium-chlor etc., and vacuum evaporation is to containing Vanadium Pentoxide in FLAKES 35%～50% at 80kPa, 70 ℃, drying temperature is 80 ℃; In the time adopting 54% strong phosphoric acid, temperature of reaction is generally at 32 ℃ and reacts 1h, and must be through secondary crystal; In addition, in phosphoric acid, conventionally also can add milk of lime etc. to purify; Visible, Ureaphil product of the prior art exists the shortcoming that complex process, purity are not high.Affect the mol ratio (n (CO (NH that the synthetic factor of Ureaphil mainly contains temperature of reaction, reaction times and urea and phosphoric acid
2)
2): n (H
3pO
4)), and the mass concentration of phosphoric acid by wet process requires to be controlled at 40%～50% in the prior art.The present invention does not directly adopt Ureaphil product as intermediate, but obtain Ureaphil that purity is higher as intermediate with phosphoric acid by wet process and urea reaction, so not only improve the purity of Ureaphil, avoid the impact of additive on Ureaphil quality product, also improved production efficiency, guarantee the supply of intermediate, save production cost, and improve production technique circuit and the parameter of Ureaphil product in prior art, obtain highly purified Ureaphil as intermediate, guaranteed the purity of SODIUM PHOSPHATE, MONOBASIC.Commercially available Ureaphil product is because period of storage is long and be subject to the reasons such as such environmental effects, its chemical property may be affected, directly utilize its raw material as production SODIUM PHOSPHATE, MONOBASIC, may affect the quality of SODIUM PHOSPHATE, MONOBASIC product, be unfavorable for the stable of quality product.
SODIUM PHOSPHATE, MONOBASIC product of the present invention both can be AMSP (NaH
2pO
4), be white crystalline powder, be convenient to store; Also can be two hypophosphite monohydrate sodium dihydrogen (NaH
2pO
42H
2o), physical and chemical index is as shown in table 1.SODIUM PHOSPHATE, MONOBASIC (Monobasic sodiumphosphate) also claim monosodium phosphate, the first sodium phosphate, is colourless column crystallization, odorless, and slightly deliquescence, soluble in water, be insoluble to ethanol, be dried to and lose whole crystal water and obtain AMSP.
The physical and chemical index of table 1 SODIUM PHOSPHATE, MONOBASIC product
| Project | Standard |
| Outward appearance | Colourless or white crystals |
| Content (dihydrate, %) | ≥98 |
| Water-insoluble (%) | ≤0.05 |
| Muriate (in Cl, %) | ≤0.014 |
| Fluorochemical (in F, %) | ≥0.005 |
| Vitriol is (with SO 2 -4Meter, %) | ≤0.25 |
| Arsenic (in As, mg/kg) | ≤3 |
| Heavy metal (in Pb, mg/kg) | ≤10 |
Beneficial effect of the present invention: operational path is short, energy consumption is low, constant product quality, production cost are low, easy to operate, production safety, carboxamide in slip is recyclable recycling also, realize cleaner production, make in whole production process environment-protecting clean pollution-free, without waste gas, waste water and waste sludge discharge, the policy that has responded energy-saving and emission-reduction, cleaner production is called, the problems such as complex process, unstable product quality, energy consumption that prior art exists are high, environmental pollution are overcome, SODIUM PHOSPHATE, MONOBASIC product purity >=98% obtaining.The present invention uses cheap carboxamide and phosphoric acid by wet process to substitute expensive thermal phosphoric acid or purifying phosphoric acid, prepares highly purified intermediate, has reached the object of purifying phosphoric acid; Intermediate is reacted to preparation SODIUM PHOSPHATE, MONOBASIC with sodium hydroxide or sodium carbonate again, compared with prior art, not only reduced resource consumption, reduced the production cost of SODIUM PHOSPHATE, MONOBASIC simultaneously, economic benefit is high.It is raw material that the present invention adopts phosphoric acid by wet process, is suitable for phosphorous chemical industry enterprise, is particularly suited for the phosphorous chemical industry enterprise with Wet-process Phosphoric Acid Production phosphorus ammonium.
Accompanying drawing explanation
Fig. 1 is equipment flowsheet of the present invention;
In figure: 1-phosphoric acid by wet process whizzer, 2-intermediate synthesizes groove, 3-intermediate crystallisation by cooling groove, 4-intermediate whizzer, 5-intermediate storage warehouse, 6-SODIUM PHOSPHATE, MONOBASIC is synthesized groove, 7-SODIUM PHOSPHATE, MONOBASIC crystallisation by cooling groove, 8-SODIUM PHOSPHATE, MONOBASIC whizzer.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with drawings and Examples, the present invention is described in further detail, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.
Fig. 1 is equipment flowsheet of the present invention, as shown in Figure 1, the present invention sends into phosphoric acid by wet process in phosphoric acid by wet process whizzer 1, to carry out removal of impurities and obtain phosphoric acid, deliver to afterwards the synthetic groove 2 of intermediate and carry out building-up reactions with carboxamide, gains are sent in intermediate crystallisation by cooling groove 3 and are carried out crystallisation by cooling, obtain intermediate through intermediate whizzer 4 centrifugal treating again, and it is interior for subsequent use to send into intermediate storage warehouse 5; Intermediate and sodium hydroxide are sent in the synthetic groove 6 of SODIUM PHOSPHATE, MONOBASIC and carried out building-up reactions, then through the crystallisation by cooling processing of SODIUM PHOSPHATE, MONOBASIC crystallisation by cooling groove 7, and the centrifugal treating of SODIUM PHOSPHATE, MONOBASIC whizzer 8, SODIUM PHOSPHATE, MONOBASIC product obtained; The centrifugal slip obtaining returns in the synthetic groove 2 of intermediate and recycles, the filtrate that intermediate whizzer 4 centrifugal treating obtain can be delivered to the raw material of composite fertilizer production line as production composite fertilizer, to realize recycle, environmental protection without the process for cleanly preparing discharging.
(1) removal of impurities of phosphoric acid by wet process:
Adopting method centrifugal or press filtration to remove concentration is the solid impurity containing in 15% phosphoric acid by wet process, obtains phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 60 ℃, under agitation condition, add carboxamide and phosphoric acid to carry out building-up reactions, the add-on of carboxamide is that 1.0:1 determines by the mol ratio of itself and phosphoric acid, stirring and dissolving insulation reaction, and the reaction times is 80min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove, and to be cooled to temperature be 20 ℃ of crystallizations, separates out rear centrifugation, retains filter cake, and filter cake is intermediate, puts into intermediate warehouse, for subsequent use; The phosphoric acid mother liquor that filtrate being contained a certain amount of impurity, is delivered to the raw material of phosphorus-ammonium compound fertilizer device as production composite fertilizer;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add a certain amount of water, under whipped state, it is dissolved completely, slowly add the sodium hydrate solid hybrid reaction of metering, the mol ratio of described intermediate and sodium hydroxide is 1:1, that controls sodium hydroxide adds speed to regulate the temperature of synthesizing in groove at 50 ℃, stirring reaction 60min; After reaction finishes, it is 20 ℃ that SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide reclaims carboxamide wherein, return to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, and quality product reaches PHOSPHORIC ACID TECH.GRADE sodium dihydrogen acceptable end product standard, dry rear packing.
(1) removal of impurities of phosphoric acid by wet process:
Adopting method centrifugal or press filtration to remove concentration is the solid impurity containing in 40% phosphoric acid by wet process, obtains phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 70 ℃, under agitation condition, add carboxamide and phosphoric acid to carry out building-up reactions, the add-on of carboxamide is that 1.05:1 determines by the mol ratio of itself and phosphoric acid, stirring and dissolving insulation reaction, and the reaction times is 100min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove, and to be cooled to temperature be 30 ℃, and centrifugation retains filter cake, and filter cake is intermediate, puts into intermediate warehouse, for subsequent use; The phosphoric acid mother liquor that filtrate being contained a certain amount of impurity, is delivered to phosphorus-ammonium compound fertilizer device;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate solid is sent in synthetic groove, add the sodium hydroxide solution of metering, hybrid reaction, the mol ratio of described intermediate and sodium hydroxide is 1.1:1, that controls sodium hydroxide solution adds speed to regulate the temperature of synthesizing in groove at 40 ℃, stirring reaction 100min; After reaction finishes, it is 30 ℃ that SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide reclaims carboxamide wherein, return to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, and quality product reaches PHOSPHORIC ACID TECH.GRADE sodium dihydrogen acceptable end product standard, dry rear packing.
(1) removal of impurities of phosphoric acid by wet process:
Adopting method centrifugal or press filtration to remove concentration is the solid impurity containing in 50% phosphoric acid by wet process, obtains phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 80 ℃, under agitation condition, add carboxamide and phosphoric acid to carry out building-up reactions, the add-on of carboxamide is that 0.95:1 determines by the mol ratio of itself and phosphoric acid, stirring and dissolving insulation reaction, and the reaction times is 60min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove, and to be cooled to temperature be 10 ℃, and centrifugation retains filter cake, and filter cake is intermediate, and intermediate is CO (NH
2)
2h
3pO
4, put into intermediate warehouse, for subsequent use; The phosphoric acid mother liquor that filtrate being contained a certain amount of impurity, is delivered to phosphorus-ammonium compound fertilizer device;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add a certain amount of water, under whipped state, it is dissolved completely, slowly add the sodium hydroxide solution hybrid reaction of metering, the mol ratio of described intermediate and sodium hydroxide is 1.2:1, that controls sodium hydroxide solution adds speed to regulate the temperature of synthesizing in groove at 70 ℃, stirring reaction 40min; After reaction finishes, it is 20 ℃ that SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide reclaims carboxamide wherein, return to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, and quality product reaches PHOSPHORIC ACID TECH.GRADE sodium dihydrogen acceptable end product standard, dry rear packing.
(1) removal of impurities of phosphoric acid by wet process:
Adopting method centrifugal or press filtration to remove concentration is the solid impurity containing in 75% phosphoric acid by wet process, obtains phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 50 ℃, under agitation condition, add carboxamide and phosphoric acid to carry out building-up reactions, the add-on of carboxamide is that 0.9:1 determines by the mol ratio of itself and phosphoric acid, stirring and dissolving insulation reaction, and the reaction times is 40min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove, and to be cooled to temperature be 0 ℃, and centrifugation retains filter cake, and filter cake is intermediate, and intermediate is CO (NH
2)
2h
3pO
4, put into intermediate warehouse, for subsequent use; The phosphoric acid mother liquor that filtrate being contained a certain amount of impurity, is delivered to phosphorus-ammonium compound fertilizer device;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add the sodium hydroxide of metering, add a certain amount of water, under whipped state, it is dissolved completely, hybrid reaction, the mol ratio of described intermediate and sodium hydroxide is 1.05:1, and that controls sodium hydroxide adds speed to regulate the temperature of synthesizing in groove at 80 ℃, stirring reaction 20min; After reaction finishes, it is 0 ℃ that SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide reclaims carboxamide wherein, return to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, and quality product reaches PHOSPHORIC ACID TECH.GRADE sodium dihydrogen acceptable end product standard, dry rear packing.
(1) removal of impurities of phosphoric acid by wet process:
Adopting method centrifugal or press filtration to remove concentration is the solid impurity containing in 52% phosphoric acid by wet process, obtains phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 40 ℃, under agitation condition, add the carboxamide reclaiming in the slip producing after sodium carbonate and intermediate reaction from step (4), carry out building-up reactions with phosphoric acid, the add-on of carboxamide is that 0.9:1 determines by the mol ratio of itself and phosphoric acid, stirring and dissolving insulation reaction, the reaction times is 120min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove and be cooled to temperature and be-10 ℃, centrifugation, retains filter cake, and filter cake is intermediate, puts into intermediate warehouse, for subsequent use; The phosphoric acid mother liquor that filtrate being contained a certain amount of impurity, is delivered to phosphorus-ammonium compound fertilizer device;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add a certain amount of water, under whipped state, it is dissolved completely, add the sodium carbonate hybrid reaction of metering, the mol ratio of described intermediate and sodium carbonate is 2.0:1, that controls sodium carbonate adds speed to regulate the temperature of synthesizing in groove at 40 ℃, stirring reaction 80min; After reaction finishes, SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature for-10 ℃, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide reclaims carboxamide wherein, return to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, and quality product reaches PHOSPHORIC ACID TECH.GRADE sodium dihydrogen acceptable end product standard, dry rear packing.
(1) removal of impurities of phosphoric acid by wet process:
Adopting method centrifugal or press filtration to remove concentration is the solid impurity containing in 52% phosphoric acid by wet process, obtains phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 90 ℃, under agitation condition, add the carboxamide reclaiming in the slip producing after sodium carbonate and intermediate reaction from step (4), carry out building-up reactions with phosphoric acid, the add-on of carboxamide is that 1.0:1 determines by the mol ratio of itself and phosphoric acid, stirring and dissolving insulation reaction, the reaction times is 60min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove, and to be cooled to temperature be 40 ℃, and centrifugation retains filter cake, and filter cake is intermediate, puts into intermediate warehouse, for subsequent use; The phosphoric acid mother liquor that filtrate being contained a certain amount of impurity, is delivered to phosphorus-ammonium compound fertilizer device;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add a certain amount of water, under whipped state, it is dissolved completely, add the sodium carbonate hybrid reaction of metering, the mol ratio of described intermediate and sodium carbonate is 2.05:1, that controls sodium carbonate adds speed to regulate the temperature of synthesizing in groove at 90 ℃, stirring reaction 20min; After reaction finishes, it is 40 ℃ that SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide reclaims carboxamide wherein, return to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, and quality product reaches PHOSPHORIC ACID TECH.GRADE sodium dihydrogen acceptable end product standard, dry rear packing.
Claims (10)
1. a method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process, is characterized in that: be to utilize carboxamide and wet-process phosphoric acid reaction to obtain intermediate, then this intermediate reacted to preparation SODIUM PHOSPHATE, MONOBASIC product with sodium hydroxide.
2. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 1, is characterized in that: comprise the following steps:
(1) removal of impurities of phosphoric acid by wet process:
Adopt method centrifugal or press filtration to remove the solid impurity containing in phosphoric acid by wet process, obtain phosphoric acid, for subsequent use;
(2) building-up reactions of intermediate:
Step (1) gained phosphoric acid is put into the synthetic groove of intermediate, regulate phosphoric acid concentration, be heated to 40 ℃-90 ℃, under agitation condition, add carboxamide and phosphoric acid to carry out building-up reactions, the add-on of carboxamide is (0.9-1.05) by it with the mol ratio of phosphoric acid: 1 is definite, and the reaction times is 40min-120min;
(3) crystallisation by cooling obtains intermediate:
After building-up reactions finishes, the intermediate slip obtaining is put into crystallisation by cooling groove and be cooled to temperature≤40 ℃, centrifugation, retains filter cake, and filter cake is intermediate, puts into intermediate warehouse, for subsequent use;
(4) preparation of SODIUM PHOSPHATE, MONOBASIC:
Intermediate is sent in synthetic groove, add the sodium hydroxide hybrid reaction of metering, the mol ratio of described intermediate and sodium hydroxide is (1-1.2): 1, and that controls sodium hydroxide adds speed to regulate the temperature of synthesizing in groove within the scope of 40 ℃-90 ℃, stirring reaction 20min-100min; After reaction finishes, SODIUM PHOSPHATE, MONOBASIC slip is cooled to temperature≤40 ℃, crystallisation by cooling, crystal is put into whizzer centrifugation after separating out, the slip that filtrate being contained carboxamide, reclaims carboxamide wherein, returns to the synthetic groove of intermediate of step (2) for the production of intermediate, filter cake is SODIUM PHOSPHATE, MONOBASIC product, dry rear packing.
3. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: the intermediate in described step (2) is CO (NH
2)
2h
3pO
4.
4. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: in described step (1), phosphoric acid by wet process concentration is 15%-75%.
5. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: after carboxamide being formulated as to carbon amide solution in described step (2), carry out building-up reactions again with phosphoric acid.
6. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: in described step (3), centrifugation gained filtrate is the intermediate slip that contains impurity, delivers to composite fertilizer production line production composite fertilizer.
7. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: in described step (4), dissolution of sodium hydroxide is obtained reacting with intermediate solid after sodium hydroxide solution.
8. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: in described step (4), dissolution of sodium hydroxide is obtained to dissolve with intermediate the solution obtaining after sodium hydroxide solution and react.
9. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: in described step (4), intermediate is dissolved to the solution obtaining and react with sodium hydrate solid.
10. a kind of method of preparing SODIUM PHOSPHATE, MONOBASIC with phosphoric acid by wet process according to claim 2, is characterized in that: described step (4) Raw sodium hydroxide is replaceable is sodium carbonate, and the mol ratio of described intermediate and sodium carbonate is (2.0～2.05): 1.
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