CN104151203B - A kind of method of vacuum evaporating crystalization continuous seepage Ureaphil - Google Patents
A kind of method of vacuum evaporating crystalization continuous seepage Ureaphil Download PDFInfo
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- CN104151203B CN104151203B CN201410340763.0A CN201410340763A CN104151203B CN 104151203 B CN104151203 B CN 104151203B CN 201410340763 A CN201410340763 A CN 201410340763A CN 104151203 B CN104151203 B CN 104151203B
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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 kind of method utilizing vacuum evaporating crystalization continuous seepage Ureaphil.The step of the method is as follows: (1) is with P
2o
5meter mass percent concentration be 40% ~ 61.9% phosphoric acid and urea be raw material, phosphoric acid and urea add in jacketed reactor continuously by 1 ︰ 1.0 ~ 1.3 mol ratio, stirring reaction, be heated to 80 ~ 90 DEG C, reaction 40 ~ 70min, material proportion is 1.4 ~ 1.6Kg/L, and material is cooled to 70 ~ 80 DEG C in dashpot, then material is carried out crystallization by plural serial stage vacuum-evaporation cooling crystallizer, then crystal solution is separated dry Ureaphil; Being separated a mother liquor part returns in jacketed reactor, and a part is for the production of wood fire retardant or fertilizer.Present invention achieves continuous crystallisation operation, solve the crystal fouling in crystallisation process, crystallization time is short, and product yield is high, and technique is simple, energy consumption is low, less investment.
Description
Technical field
The present invention relates to the derivative of urea, relate in particular to a kind of method of vacuum evaporating crystalization continuous seepage Ureaphil.
Background technology
Ureaphil is a kind of ligand complex compound with amino structure generated by phosphoric acid and urea reaction, is a kind of fine chemical product being widely used in the fields such as livestock industry, agricultural, industry.It is a kind of excellent fodder additives, for livestock provides phosphorus and non-protein nitrogen(NPN) (urea nitrogen) two kinds of nutritive elements; Or a kind of high concentration N phosphorus composite fertilizer, be applicable to alkaline soil, carry out test in China some areas to Ureaphil solid fertilizer to prove: the effect that Ureaphil has had crop growth, not only can ensure the normal growth of plant, and does not have negative impact to soil; 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 DEG C, Wood products after ammonium polyphosphate process can 210 DEG C time 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; Also can be used as fire prevention clean-out system and the granular fire-fighting medium of preparation etc.Especially as the legal I class additive of the European Community (FAO) feed industry, 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 current production 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 preferentially separated out at the lower crystallizer inwall of temperature or coil pipe outside surface due to crystal, 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), the production cycle is caused to extend, productive rate declines, and needs regularly to remove brilliant dirt, and production cost increases.
Summary of the invention
The object of the invention is to overcome above-mentioned shortcoming, a kind of method of vacuum evaporating crystalization continuous seepage Ureaphil is provided, solves the crystal fouling in crystallisation process, achieve continuous crystallisation operation and produce.
Technical scheme of the present invention is: a kind of method of vacuum evaporating crystalization continuous seepage Ureaphil, and the step of the method is as follows:
(1) with P
2o
5meter mass percent concentration be 40% ~ 61.9% phosphoric acid and urea add continuously in jacketed reactor by 1 ︰ 1.0 ~ 1.3 mol ratio, stirring reaction, rotating speed is 50 ~ 60rpm, is heated to 80 ~ 90 DEG C, react 40 ~ 70min, material proportion is 1.4 ~ 1.6Kg/L;
(2) by material dashpot medium speed be 50 ~ 60rpm stir, cool to 70 ~ 80 DEG C, then material is carried out crystallization by thtee-stage shiplock band stirring vacuum transpiration cooling crystallizer, mixing speed is 20 ~ 50rpm, first step vacuum tightness is 0.06 ~ 0.07MPa, and temperature of charge is down to 58 ~ 68 DEG C; Second stage vacuum tightness is 0.07 ~ 0.08MPa, and temperature of charge is down to 48 ~ 58 DEG C; Third stage vacuum tightness is 0.08 ~ 0.09MPa, and temperature of charge is down to 40 ~ 50 DEG C; Again by crystal solution separation, drying, obtain Ureaphil product;
(3) be separated mother liquor 20 ~ 40% and return jacketed reactor for the production of Ureaphil, 60 ~ 80% for the production of wood fire retardant or fertilizer.
When adopting aforesaid method first time to produce, 0.1 ~ 0.8% Ureaphil crystal seed of quality of material need be added 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, solve the crystal fouling in crystallisation process, crystallization time shortens, and product yield is high, and achieve continuous crystallisation and produce, improve plant capacity, the plant running cycle is long; Mother liquor 20 ~ 40% after separation returns jacketed reactor for the production of Ureaphil, and 60 ~ 80% for the production of wood fire retardant or fertilizer, solves 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-first degree crystalline device; 4-secondary crystallizer; 5-tri-grades of crystallizers; 6-whizzer; 7-drying machine; 8-thermal medium; 9-coolant media.
Embodiment
embodiment 1
As shown in Figure 1, P
2o
5mass percent concentration be 40% phosphoric acid join in 1000L jacketed reactor with 400Kg/h, and open stirring, rotating speed is 50rpm, add urea with 176Kg/h simultaneously, be warming up to 80 DEG C, 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 DEG C 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 DEG C, enter second stage vacuum-evaporation cooling crystallizer again and carry out crystallization, mixing speed is 20rpm, vacuum tightness is 0.07MPa, temperature of charge is down to 48 DEG C, 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 DEG C, again by crystal solution separation, drying, obtain Ureaphil product (after testing, P
2o
544.56%, N17.53%).
embodiment 2
As shown in Figure 1, P
2o
5mass percent concentration be 44% phosphoric acid join in 1000L jacketed reactor with 400Kg/h, and open stirring, rotating speed is 50rpm, add urea with 178Kg/h simultaneously, be warming up to 85 DEG C, 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 DEG C 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 DEG C, enter second stage vacuum-evaporation cooling crystallizer again and carry out crystallization, mixing speed is 30rpm, vacuum tightness is 0.075MPa, temperature of charge is down to 53 DEG C, 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 DEG C, again by crystal solution separation, drying, obtain Ureaphil product (after testing, P
2o
544.72%, N17.09%).
embodiment 3
As shown in Figure 1, P
2o
5mass percent concentration be 55% phosphoric acid join in 1000L jacketed reactor with 400Kg/h, and open stirring, rotating speed is 55rpm, add urea with 204Kg/h simultaneously, be warming up to 85 DEG C, 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 DEG C 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 DEG C, enter second stage vacuum-evaporation cooling crystallizer again and carry out crystallization, mixing speed is 40rpm, vacuum tightness is 0.08MPa, temperature of charge is down to 53 DEG C, 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 DEG C, again by crystal solution separation, drying, obtain Ureaphil product (after testing, P
2o
544.65%, N17.53%).
embodiment 4
As shown in Figure 1, P
2o
5mass percent concentration be 61.9% phosphoric acid join in 1000L jacketed reactor with 400Kg/h, and open stirring, rotating speed is 60rpm, add urea with 209Kg/h simultaneously, be warming up to 90 DEG C, 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 DEG C 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 DEG C, enter second stage vacuum-evaporation cooling crystallizer again and carry out crystallization, mixing speed is 50rpm, vacuum tightness is 0.08MPa, temperature of charge is down to 58 DEG C, 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 DEG C, again by crystal solution separation, drying, obtain Ureaphil product (after testing, P
2o
544.72%, N17.40%).
Claims (2)
1. a method for vacuum evaporating crystalization continuous seepage Ureaphil, is characterized in that: the step of the method is as follows:
(1) with P
2o
5meter mass percent concentration be 40% ~ 61.9% phosphoric acid and urea add continuously in jacketed reactor by 1:1.0 ~ 1.3 mol ratio, stirring reaction, rotating speed is 50 ~ 60rpm, is heated to 80 ~ 90 DEG C, react 40 ~ 70min, material proportion is 1.4 ~ 1.6Kg/L;
(2) by material dashpot medium speed be 50 ~ 60rpm stir, cool to 70 ~ 80 DEG C, then material is carried out crystallization by thtee-stage shiplock band stirring vacuum transpiration cooling crystallizer, mixing speed is 20 ~ 50rpm, first step vacuum tightness is 0.06 ~ 0.07MPa, and temperature of charge is down to 58 ~ 68 DEG C; Second stage vacuum tightness is 0.07 ~ 0.08MPa, and temperature of charge is down to 48 ~ 58 DEG C; Third stage vacuum tightness is 0.08 ~ 0.09MPa, and temperature of charge is down to 40 ~ 50 DEG C; Again by crystal solution separation, drying, obtain Ureaphil product;
(3) be separated mother liquor 20 ~ 40% and return jacketed reactor for the production of Ureaphil, 60 ~ 80% for the production of wood fire retardant or fertilizer.
2. the method for a kind of vacuum evaporating crystalization continuous seepage Ureaphil according to claim 1, is characterized in that: first time produces, and need add 0.1 ~ 0.8% Ureaphil crystal seed of quality of material in dashpot.
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| 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 |
| 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 |
| 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 |
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 |
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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 |
|---|
| 多级结晶器的有效能分析与最佳化;王静康 等;《天津大学学报》;19851231(第3期);摘要，第55页最后1段至第56页第1段 * |
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