CN102040544A - Method for continuously producing feed grade urea phosphate by using wet purified phosphoric acid - Google Patents

Method for continuously producing feed grade urea phosphate by using wet purified phosphoric acid Download PDF

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Publication number
CN102040544A
CN102040544A CN2010105439958A CN201010543995A CN102040544A CN 102040544 A CN102040544 A CN 102040544A CN 2010105439958 A CN2010105439958 A CN 2010105439958A CN 201010543995 A CN201010543995 A CN 201010543995A CN 102040544 A CN102040544 A CN 102040544A
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China
Prior art keywords
phosphoric acid
feed grade
vacuum concentration
ureaphil
purified phosphoric
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Pending
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CN2010105439958A
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Chinese (zh)
Inventor
毛克万
梅胜明
周佩
张志平
陈鹏
姜贵华
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Sinochem Fuling Chongqing Chemical Industry Co Ltd
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Sinochem Fuling Chongqing Chemical Industry Co Ltd
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Priority to CN2010105439958A priority Critical patent/CN102040544A/en
Publication of CN102040544A publication Critical patent/CN102040544A/en
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Abstract

The invention discloses a method for continuously producing feed grade urea phosphate by using wet purified phosphoric acid, which is characterized by comprising the following steps of: continuously adding 5 to 7 percent wet purified phosphoric acid and urea according to a molar ratio of 1:(1.0-1.05) for mixing, reacting with stirring at the temperature of between 70 and 85 DEG C for 30 to 60 minutes, keeping the temperature of between 80 and 90 DEG C, performing vacuum concentration under the pressure of between 33 and 38Kp, concentrating materials, crystallizing and cooling to the temperature of 35 DEG C, separating and drying crystalline liquid to obtain the feed grade urea phosphate, and returning mother liquor to the vacuum concentration. In the method, the urea phosphate is continuously produced by taking the purified phosphoric acid on the basis of wet extraction purification technology as a raw material, namely the purified phosphoric acid and the urea are directly taken as raw materials, and are subjected to heating, vacuum concentration, cooling crystallization, separation and drying to obtain a feed grade urea phosphate product, and an active agent, a suspending agent and the like are not required to be added in the reaction, so that the reaction process is simple, and high in continuity, yield and product purity, ensures that the mother liquid is not generated, and has high promotional value for the subsequent product development of the purified phosphoric acid.

Description

Method with wet purification phosphoric acid continuous production feed grade Ureaphil
Technical field
The invention belongs to the phosphorus chemistry industrial circle, specifically, relating to a kind of is the method for raw material continuous production Ureaphil with wet purification phosphoric acid.
Background technology
The phosphoric acid arteries and veins is mainly used in the cattle and sheep class instead from the fodder additives of animal as a kind of useful fine chemical product, in addition also as the silage preserving agent, high concentration N, phosphorus composite fertilizer, the ammonium polyphosphate intermediate, fire retardant, fire prevention clean-out systems etc., its application relates to fields such as livestock industry, industry, agricultural, has vast market prospect.
The domestic production Ureaphil is many at present is raw material with the thermal phosphoric acid, carry out producing after the removal of impurities, and its production cost height, product price is higher.Domestic also have big quantity research and partial monopoly to the Wet-process Phosphoric Acid Production Ureaphil, but what adopt all is that the strong phosphoric acid of chemical fertilizers production is a raw material, and the constantly removal of impurity is added various reaction promotors simultaneously and just can be carried out in the production process.Because many content of dopant species height in the raw material phosphoric acid can't eliminate impurity, the Ureaphil purity of its production is all not really high, only can reach agriculture grade standard.
Summary of the invention
For solving above technical problem, the object of the present invention is to provide a kind of continuously, the method for low-cost, cleaner production feed grade Ureaphil.
The present invention seeks to realize like this:
A kind of method with wet purification phosphoric acid continuous production feed grade Ureaphil, its key is: add mixing with 5%~70% wet purification phosphoric acid and urea continuously by 1:1.0~1.05 molar ratios, under 70~85 ℃ condition, stirring reaction 30~60min, holding temperature is 80~90 ℃ then, and pressure is vacuum concentration under the vacuum condition of 33~38Kp, and material concentrates post crystallization and is cooled to 35 ℃, crystal solution is separated drying obtain the feed grade Ureaphil, mother liquor turns back to vacuum concentration.Vacuum concentration in the step evaporates large quantity of moisture, can improve last yield, after handling through this vacuum concentration simultaneously, crystal solution is separated drying and is obtained the feed grade Ureaphil, and remaining mother liquor can turn back to vacuum concentration, realizes continuous production concentrated mother liquor circulation crystallization.Can be with its emission treatment.
As optimization, above-mentioned wet purification phosphoric acid and urea are in chuck heating-type reaction kettle for reaction, and mixing speed is 65~200 commentaries on classics/min.The vacuum concentration of material carries out in the vacuum concentration still, and the crystallization of described material and cooling are carried out in oslo cooler crystallizer.Crystal solution is separated drying and is obtained the feed grade Ureaphil, and mother liquor turns back to the vacuum concentration still and carries out vacuum concentration.Above-mentioned reaction is not got rid of and is utilized other equipment to carry out identical processing.
Beneficial effect:
Present method is that raw material continuous production Ureaphil is to be raw material with purifying phosphoric acid and urea directly based on the purifying phosphoric acid of liquid extraction purification techniques, reacting by heating, vacuum concentration, decrease temperature crystalline, separation, the dry feed grade Ureaphil product that gets need not to add activator and suspension agent etc. in the reaction.Make reaction process simple, continuity is good, the yield height, and the product purity height, no mother liquor effluxes, and exploitation has higher promotional value to the subsequent product of purifying phosphoric acid.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1
As shown in Figure 1, starting whipping appts is 31% with 300kg/h(concentration) wet purification phosphoric acid joins in the 500L jacketed type reactor, the heating of wet purification phosphoric acid temperature is maintained 70 ℃, add 62kg/h urea simultaneously, reacted feed liquid overflows to 500L vacuum concentration still, be controlled under the vacuum condition that pressure is 38Kpa, keep the concentration kettle temperature at 80 ℃, material after concentrating is put into Oslo crystallizer and is cooled to 35 ℃ of crystallizations, crystal solution is dry through separating, drying temperature is controlled at 110 ℃, obtains the average 148kg/h of product, and yield is 98.7%.
Embodiment 2
As shown in Figure 1, starting whipping appts is 31% with 300kg/h(concentration) wet purification phosphoric acid joins in the 500L jacketed type reactor, the heating of wet purification phosphoric acid temperature is maintained 85 ℃, add 62kg/h urea simultaneously, reacted feed liquid overflows to 500L vacuum concentration still, be controlled under the vacuum condition that pressure is 33Kpa, keep the concentration kettle temperature at 90 ℃, material after concentrating is put into Oslo crystallizer and is cooled to 35 ℃ of crystallizations, crystal solution is dry through separating, drying temperature is controlled at 100 ℃, and obtaining product, to record yield be 98.8%.
Embodiment 3
As shown in Figure 1, starting whipping appts is 70% with 300kg/h(concentration) wet purification phosphoric acid joins in the 500L jacketed type reactor, the heating of wet purification phosphoric acid temperature is maintained 70 ℃, add 133kg/h urea simultaneously, mixing speed is 65 commentaries on classics/min, keep the chuck temperature of reaction kettle at 70 ℃, the residence time is 60min, and reacted feed liquid overflows to 500L vacuum concentration still, is controlled under the vacuum condition that pressure is 33Kpa, keep the concentration kettle temperature at 80 ℃, material after concentrating is put into Oslo crystallizer and is cooled to 35 ℃ of crystallizations, and crystal solution is dry through separating, and drying temperature is controlled at 100 ℃, obtain the average 353kg/h of product, yield 98.8%.
Embodiment 4
As shown in Figure 1, starting whipping appts is 70% with 300kg/h(concentration) wet purification phosphoric acid joins in the 500L jacketed type reactor, the heating of wet purification phosphoric acid temperature is maintained 80 ℃, add 133kg/h urea simultaneously, mixing speed is 200 commentaries on classics/min, keep the chuck temperature of reaction kettle at 85 ℃, the residence time is 30min, reacted feed liquid overflows to 500L vacuum concentration still, is controlled under the vacuum condition that pressure is 38Kpa, keeps the concentration kettle temperature at 90 ℃, material after concentrating is put into Oslo crystallizer and is cooled to 35 ℃ of crystallizations, crystal solution is dry through separating, and drying temperature is controlled at 110 ℃, obtains product and records yield 98.9%.

Claims (4)

1. method with wet purification phosphoric acid continuous production feed grade Ureaphil, it is characterized in that: add mixing continuously by 1:1.0~1.05 molar ratios with 5%~70% wet purification phosphoric acid and urea, under 70~85 ℃ condition, stirring reaction 30~60min, holding temperature is 80~90 ℃ then, is vacuum concentration under the vacuum condition of 33~38Kp at pressure, and material concentrates post crystallization and is cooled to 35 ℃, crystal solution is separated drying obtain the feed grade Ureaphil, mother liquor turns back to vacuum concentration.
2. according to the described method with wet purification phosphoric acid continuous production feed grade Ureaphil of claim 1, it is characterized in that: described wet purification phosphoric acid and urea are in chuck heating-type reaction kettle for reaction, and mixing speed is 65~200 commentaries on classics/min.
3. according to claim 1 or 2 described methods with wet purification phosphoric acid continuous production feed grade Ureaphil, it is characterized in that: the vacuum concentration of described material carries out in the vacuum concentration still, and the crystallization of described material and cooling are carried out in oslo cooler crystallizer.
4. according to the described method with wet purification phosphoric acid continuous production feed grade Ureaphil of claim 3, it is characterized in that: described crystal solution is separated drying and is obtained the feed grade Ureaphil, and mother liquor turns back to the vacuum concentration still and carries out vacuum concentration.
CN2010105439958A 2010-11-15 2010-11-15 Method for continuously producing feed grade urea phosphate by using wet purified phosphoric acid Pending CN102040544A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102391155A (en) * 2011-10-25 2012-03-28 贵州川恒化工有限责任公司 Urea phosphate production method
CN102531709A (en) * 2012-03-09 2012-07-04 广西力源肥业科技农化有限公司 Method for industrially and continuously producing crystalline urea
CN103694143A (en) * 2013-12-25 2014-04-02 贵州开磷(集团)有限责任公司 Device for continuously producing urea phosphate from wet-process phosphoric acid
CN104045582A (en) * 2014-06-06 2014-09-17 云南云天化国际化工有限公司 Method for producing feed-grade urea phosphate from urea phosphate mother solution
CN104311181A (en) * 2014-09-19 2015-01-28 贵州大学 Preparation method of special fertilizer for honey peaches
CN105503657A (en) * 2015-12-31 2016-04-20 王丰登 Production method of urea phosphate
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
CN115304514A (en) * 2022-08-17 2022-11-08 新中天环保股份有限公司 Process for preparing urea phosphate by recycling waste phosphoric acid in photoelectric industry

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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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CN101318914A (en) * 2008-07-23 2008-12-10 瓮福(集团)有限责任公司 Method for preparing urea phosphoric acid with wet-process phosphoric acid
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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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102391155A (en) * 2011-10-25 2012-03-28 贵州川恒化工有限责任公司 Urea phosphate production method
CN102391155B (en) * 2011-10-25 2014-02-26 贵州川恒化工有限责任公司 Urea phosphate production method
CN102531709A (en) * 2012-03-09 2012-07-04 广西力源肥业科技农化有限公司 Method for industrially and continuously producing crystalline urea
CN103694143A (en) * 2013-12-25 2014-04-02 贵州开磷(集团)有限责任公司 Device for continuously producing urea phosphate from wet-process phosphoric acid
CN104045582A (en) * 2014-06-06 2014-09-17 云南云天化国际化工有限公司 Method for producing feed-grade urea phosphate from urea phosphate mother solution
CN104045582B (en) * 2014-06-06 2015-12-09 云南云天化国际化工有限公司 Utilize the method for Ureaphil mother liquor production feed grade Ureaphil
CN104311181A (en) * 2014-09-19 2015-01-28 贵州大学 Preparation method of special fertilizer for honey peaches
CN105503657A (en) * 2015-12-31 2016-04-20 王丰登 Production method of urea phosphate
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
CN115304514A (en) * 2022-08-17 2022-11-08 新中天环保股份有限公司 Process for preparing urea phosphate by recycling waste phosphoric acid in photoelectric industry
CN115304514B (en) * 2022-08-17 2023-11-14 新中天环保股份有限公司 Process for preparing urea phosphate by recycling waste phosphoric acid in photoelectric industry

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Application publication date: 20110504