CN104151203A - Method for continuously producing urea phosphate by vacuum evaporation crystallization - Google Patents
Method for continuously producing urea phosphate by vacuum evaporation crystallization Download PDFInfo
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- CN104151203A CN104151203A CN201410340763.0A CN201410340763A CN104151203A CN 104151203 A CN104151203 A CN 104151203A CN 201410340763 A CN201410340763 A CN 201410340763A CN 104151203 A CN104151203 A CN 104151203A
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- ureaphil
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention discloses a method for continuously producing urea phosphate by vacuum evaporation crystallization. The method comprises the following steps: (1) by using phosphoric acid containing 40-61.9 wt% of P2O5 and urea as raw materials, continuously adding the phosphoric acid and urea into a jacket reactor in a mole ratio of 1:(1.0-1.3), stirring to react, heating to 80-90 DEG C, reacting for 40-70 minutes, cooling the material (the specific gravity is 1.4-1.6 Kg/L) to 70-80 DEG C in a buffer tank, crystallizing the material in a multistage cascade vacuum evaporation cooling crystallizer, separating the crystallizing solution, and drying to obtain the urea phosphate, wherein part of the separated mother solution returns to the jacket reactor, and the rest is used for producing the wood flame retardant or fertilizer. The method implements continuous crystallization operation, solves the problem of crystal scales in the crystallization process, and has the advantages of short crystallization time, high product yield, simple technique, low energy consumption and low investment.
Description
Technical field
The present invention relates to the derivative of urea, relate in particular to a kind of method that vacuum evaporating crystalization is produced Ureaphil continuously.
Background technology
Ureaphil is a kind of ligand complex compound with amino structure being generated by phosphoric acid and urea reaction, is a kind of fine chemical product that is widely used in the fields such as livestock industry, agricultural, industry.It is a kind of good fodder additives, for livestock provides phosphorus and two kinds of nutritive elements of non-protein nitrogen(NPN) (urea nitrogen); Or a kind of high concentration N phosphorus composite fertilizer, be applicable to alkaline soil, in China some areas, Ureaphil solid fertilizer is carried out to evidence: the effect that Ureaphil has had crop growth, not only can guarantee the normal growth of plant, and soil is not had to negative impact; Ureaphil also can be used as ammonium polyphosphate intermediate, ammonium polyphosphate is a kind of efficient compound nitrogen phosphate fertilizer, also be a kind of widely used fire retardant simultaneously, decomposition temperature is higher than 200 ℃, Wood products can be in the time of 210 ℃ after ammonium polyphosphate is processed surface missing of ignition, therefore Ureaphil can be used for the fire-retardant finish of plank fibre product, cotton fiber product and resin, prepares refractory paint; Clean-out system and the granular fire-fighting medium of preparation etc. also can be used as preventing fires.Especially as the legal I class of the European Community (FAO) feed industry additive, the ruminating animal special nutritional additive of Food and Argriculture OrganizationFAO (FAO) recommendation and the supplement of phosphorus, have wide market outlook.
The method of producing at present Ureaphil is a lot, mainly contain dividing wall type or coil tube type crystallisation by cooling method, it all belongs to intermittent crystallization method, and these methods are because crystal is preferentially separated out at the lower crystallizer inwall of temperature or coil pipe outside surface, crystallizer inwall or coil pipe outside surface form thick crystalline substance dirt, cause heat exchange efficiency to decline, cooling is slow, crystallization time long (generally needing 6 ~ 10 hours), cause the production cycle to extend, productive rate declines, and needs regularly brilliant dirt to be removed, and production cost increases.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming, a kind of method that provides vacuum evaporating crystalization to produce continuously Ureaphil, has solved the crystal fouling in crystallisation process, has realized continuous crystallisation operation and has produced.
Technical scheme of the present invention is: a kind of vacuum evaporating crystalization is produced the method for Ureaphil continuously, and the step of the method is as follows:
(1) with P
2o
5phosphoric acid and urea that meter mass percent concentration is 40% ~ 61.9% add in jacketed reactor continuously by 1 ︰ 1.0 ~ 1.3 mol ratios, stirring reaction, and rotating speed is 50 ~ 60rpm, is heated to 80 ~ 90 ℃, reaction 40 ~ 70min, material proportion is 1.4 ~ 1.6Kg/L;
(2) by material, at dashpot medium speed, be that 50 ~ 60rpm stirs, cool to 70 ~ 80 ℃, then material is carried out to crystallization by three grades of series connection band stirring vacuum transpiration cooling crystallizers, mixing speed is 20 ~ 50rpm, first step vacuum tightness is 0.06 ~ 0.07MPa, and temperature of charge is down to 58 ~ 68 ℃; Second stage vacuum tightness is 0.07 ~ 0.08MPa, and temperature of charge is down to 48 ~ 58 ℃; Third stage vacuum tightness is 0.08 ~ 0.09MPa, and temperature of charge is down to 40 ~ 50 ℃; Again that crystal solution is separated, dry, obtain Ureaphil product;
(3) separated mother liquor 20 ~ 40% returns to jacketed reactor for the production of Ureaphil, and 60 ~ 80% for the production of wood fire retardant or fertilizer.
While adopting aforesaid method to produce for the first time, need be to 0.1 ~ 0.8% Ureaphil crystal seed that adds quality of material in dashpot.
Advantage of the present invention: method technique of the present invention is simple, energy consumption is low, less investment, easily realizes suitability for industrialized production; Because the present invention is evaporative crystallization under vacuum condition, solved the crystal fouling in crystallisation process, crystallization time shortens, and product yield is high, has realized continuous crystallisation production, has improved plant capacity, and the device cycle of operation is long; Mother liquor 20 ~ 40% after separation returns to jacketed reactor for the production of Ureaphil, and 60 ~ 80% for the production of wood fire retardant or fertilizer, has solved the problem of mother liquid recycling.Products obtained therefrom reaches the index request of fertilizer grade and feed grade Ureaphil, has very high economic benefit and social benefit.
accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
In figure: 1-jacketed reactor; 2-dashpot; 3-one-level crystallizer; 4-secondary crystallization device; Tri-grades of crystallizers of 5-; 6-whizzer; 7-drying machine; 8-thermal medium; 9-coolant media.
Embodiment
embodiment 1
As shown in Figure 1, P
2o
5mass percent concentration is that 40% phosphoric acid joins in 1000L jacketed reactor with 400Kg/h, and open and stir, rotating speed is 50rpm, with 176Kg/h, add urea simultaneously, be warming up to 80 ℃, reaction 40min, material proportion is 1.4Kg/L, feed liquid overflows to 1000L dashpot, open and stir, rotating speed is 50rpm, and be cooled to 70 ℃ by dashpot chuck cooling medium, enter first step vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 20rpm, vacuum tightness is 0.06MPa, temperature of charge is down to 58 ℃, enter again second stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 20rpm, vacuum tightness is 0.07MPa, temperature of charge is down to 48 ℃, finally enter third stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 20rpm, vacuum tightness is 0.08MPa, temperature of charge is down to 40 ℃, again that crystal solution is separated, dry, obtain Ureaphil product (P after testing,
2o
544.56%, N17.53%).
embodiment 2
As shown in Figure 1, P
2o
5mass percent concentration is that 44% phosphoric acid joins in 1000L jacketed reactor with 400Kg/h, and open and stir, rotating speed is 50rpm, with 178Kg/h, add urea simultaneously, be warming up to 85 ℃, reaction 50min, material proportion is 1.43Kg/L, feed liquid overflows to 1000L dashpot, open and stir, rotating speed is 50rpm, and be cooled to 75 ℃ by dashpot chuck cooling medium, enter first step vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 30rpm, vacuum tightness is 0.065MPa, temperature of charge is down to 63 ℃, enter again second stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 30rpm, vacuum tightness is 0.075MPa, temperature of charge is down to 53 ℃, finally enter third stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 30rpm, vacuum tightness is 0.085MPa, temperature of charge is down to 45 ℃, again that crystal solution is separated, dry, obtain Ureaphil product (P after testing,
2o
544.72%, N17.09%).
embodiment 3
As shown in Figure 1, P
2o
5mass percent concentration is that 55% phosphoric acid joins in 1000L jacketed reactor with 400Kg/h, and open and stir, rotating speed is 55rpm, with 204Kg/h, add urea simultaneously, be warming up to 85 ℃, reaction 60min, material proportion is 1.53Kg/L, feed liquid overflows to 1000L dashpot, open and stir, rotating speed is 55pm, and be cooled to 75 ℃ by dashpot chuck cooling medium, enter first step vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 40rpm, vacuum tightness is 0.07MPa, temperature of charge is down to 63 ℃, enter again second stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 40rpm, vacuum tightness is 0.08MPa, temperature of charge is down to 53 ℃, finally enter third stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 40rpm, vacuum tightness is 0.09MPa, temperature of charge is down to 45 ℃, again that crystal solution is separated, dry, obtain Ureaphil product (P after testing,
2o
544.65%, N17.53%).
embodiment 4
As shown in Figure 1, P
2o
5mass percent concentration is that 61.9% phosphoric acid joins in 1000L jacketed reactor with 400Kg/h, and open and stir, rotating speed is 60rpm, with 209Kg/h, add urea simultaneously, be warming up to 90 ℃, reaction 70min, material proportion is 1.6Kg/L, feed liquid overflows to 1000L dashpot, open and stir, rotating speed is 60pm, and be cooled to 80 ℃ by dashpot chuck cooling medium, enter first step vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 50rpm, vacuum tightness is 0.07MPa, temperature of charge is down to 68 ℃, enter again second stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 50rpm, vacuum tightness is 0.08MPa, temperature of charge is down to 58 ℃, finally enter third stage vacuum-evaporation cooling crystallizer and carry out crystallization, mixing speed is 50rpm, vacuum tightness is 0.09MPa, temperature of charge is down to 50 ℃, again that crystal solution is separated, dry, obtain Ureaphil product (P after testing,
2o
544.72%, N17.40%).
Claims (2)
1. vacuum evaporating crystalization is produced a method for Ureaphil continuously, it is characterized in that: the step of the method is as follows:
(1) with P
2o
5phosphoric acid and urea that meter mass percent concentration is 40% ~ 61.9% add in jacketed reactor continuously by 1 ︰ 1.0 ~ 1.3 mol ratios, stirring reaction, and rotating speed is 50 ~ 60rpm, is heated to 80 ~ 90 ℃, reaction 40 ~ 70min, material proportion is 1.4 ~ 1.6Kg/L;
(2) by material, at dashpot medium speed, be that 50 ~ 60rpm stirs, cool to 70 ~ 80 ℃, then material is carried out to crystallization by three grades of series connection band stirring vacuum transpiration cooling crystallizers, mixing speed is 20 ~ 50rpm, first step vacuum tightness is 0.06 ~ 0.07MPa, and temperature of charge is down to 58 ~ 68 ℃; Second stage vacuum tightness is 0.07 ~ 0.08MPa, and temperature of charge is down to 48 ~ 58 ℃; Third stage vacuum tightness is 0.08 ~ 0.09MPa, and temperature of charge is down to 40 ~ 50 ℃; Again that crystal solution is separated, dry, obtain Ureaphil product;
(3) separated mother liquor 20 ~ 40% returns to jacketed reactor for the production of Ureaphil, and 60 ~ 80% for the production of wood fire retardant or fertilizer.
2. the method that a kind of vacuum evaporating crystalization according to claim 1 is produced Ureaphil continuously, is characterized in that: produces for the first time, and need be to 0.1 ~ 0.8% Ureaphil crystal seed that adds quality of material in dashpot.
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| CN201410340763.0A CN104151203B (en) | 2014-07-17 | 2014-07-17 | A kind of method of vacuum evaporating crystalization continuous seepage Ureaphil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349116A (en) * | 2016-08-25 | 2017-01-25 | 湖北三宁化工股份有限公司 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
| CN110790685A (en) * | 2019-12-09 | 2020-02-14 | 武汉科技大学 | Method for producing urea phosphate by wet-process phosphoric acid reduced pressure evaporation coupled elution crystallization |
| CN110790684A (en) * | 2019-12-09 | 2020-02-14 | 武汉科技大学 | Method for producing urea phosphate by using wet-process phosphoric acid as raw material through elution crystallization |
| CN111004153A (en) * | 2019-12-09 | 2020-04-14 | 武汉科技大学 | Method for producing urea phosphate by using wet-process phosphoric acid as raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4461913A (en) * | 1981-11-24 | 1984-07-24 | Tennessee Valley Authority | Production of urea phosphate |
| CN101665453A (en) * | 2009-07-31 | 2010-03-10 | 瓮福（集团）有限责任公司 | Method for producing urea phosphate through vacuum crystallization |
-
2014
- 2014-07-17 CN CN201410340763.0A patent/CN104151203B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4461913A (en) * | 1981-11-24 | 1984-07-24 | Tennessee Valley Authority | Production of urea phosphate |
| CN101665453A (en) * | 2009-07-31 | 2010-03-10 | 瓮福（集团）有限责任公司 | Method for producing urea phosphate through vacuum crystallization |
Non-Patent Citations (1)
| Title |
|---|
| 王静康 等: "多级结晶器的有效能分析与最佳化", 《天津大学学报》, no. 3, 31 December 1985 (1985-12-31) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349116A (en) * | 2016-08-25 | 2017-01-25 | 湖北三宁化工股份有限公司 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
| CN110790685A (en) * | 2019-12-09 | 2020-02-14 | 武汉科技大学 | Method for producing urea phosphate by wet-process phosphoric acid reduced pressure evaporation coupled elution crystallization |
| CN110790684A (en) * | 2019-12-09 | 2020-02-14 | 武汉科技大学 | Method for producing urea phosphate by using wet-process phosphoric acid as raw material through elution crystallization |
| CN111004153A (en) * | 2019-12-09 | 2020-04-14 | 武汉科技大学 | Method for producing urea phosphate by using wet-process phosphoric acid as raw material |
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Address after: 550500 Guizhou Province, Qiannan Buyei and Miao Autonomous Prefecture Fuquan Racecourse town Yingbin Road No. 1 Wengfu group Patentee after: WENGFU GROUP Co.,Ltd. Address before: 23, 550002 floor, International Building, No. 57, South City Road, Nanming District, Guiyang, Guizhou Patentee before: WENGFU GROUP Co.,Ltd. |
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