CN106349116A - Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid - Google Patents
Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid Download PDFInfo
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- CN106349116A CN106349116A CN201610721841.0A CN201610721841A CN106349116A CN 106349116 A CN106349116 A CN 106349116A CN 201610721841 A CN201610721841 A CN 201610721841A CN 106349116 A CN106349116 A CN 106349116A
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- phosphoric acid
- urea phosphate
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- strip liquor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
- C07C273/14—Separation; Purification; Stabilisation; Use of additives
- C07C273/16—Separation; Purification
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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid. The method comprises the following steps: firstly, adding the wet-method purified phosphoric acid strip liquor or washing residual liquid of which the concentration of P2O5 is 25-40% into a reaction tank, controlling the temperature to be 60-85 DEG C, stirring at a speed of 100-200r/min, keeping the temperature for 10-20 minutes, adding urea into the reaction tank in a mole ratio of phosphoric acid to urea of 1:(1.0-1.2), performing a stirring reaction for 60-90 minutes, and concentrating reaction liquid under a vacuum condition to increase the concentration of P2O5 to be 48-55%, so as to form a concentrated reactant material; reducing the temperature of the concentrated reactant material to be 5-40 DEG C, adding a crystal seed, and performing cooling constant-temperature crystallization under a stirring condition of 5-30r/min so as to separate urea phosphate; and performing centrifugal separation on the urea phosphate, and drying, thereby obtaining the feed-grade urea phosphate. The production cost is relatively low when being compared with that of industrial phosphoric acid or hot-method phosphoric acid, no activating agent, suspending agent and the like are needed in the production process, the process procedures are simple, and relatively high economic and environment-friendly values can be made.
Description
Technical field
The invention belongs to phosphorous chemical industry field and in particular to one kind purifying phosphoric acid strip liquor or scrub raffinate continuously produce in a wet process
The method of urea phosphate.
Background technology
Urea phosphate, chemical formula is co (nh2)2.h3po4, n content is 17.7%, p2o5Content is 44.9%, aqueous solution
In acidity.It is a kind of important fine inorganic chemicals product, all has and have been widely used and prospect in agricultural and industry, bag
Include ensilage preserving agent, high concentration N-phosphorus composite fertilizer, APP intermediate, fire retardant and fire prevention abluent etc., especially
It is the feed additive as ruminant, yield and the quality of ruminant meat and milk can be significantly improved.
At present, domestic production of urea phosphate is how based on thermal phosphoric acid and phosphoric acid by wet process.Thermal phosphoric acid yield is higher, but cost
High, production capacity is little；Both at home and abroad phosphoric acid by wet process is studied for raw material production urea phosphate, but in phosphoric acid by wet process, impurity is more, special
It is not f-、so4 2-、al3+And fe3+There is large effect Deng to urea phosphate product yield and purity, using no purification of wet process phosphoric acid
The urea phosphate product purity producing is not high, generally needed to be added activator, and Recycling Mother Solution is difficult, is used for producing fertilizer phosphorus
Sour urea；If it is relatively costly directly to produce urea phosphate with 75% or 85% purifying phosphoric acid, and general strip liquor need to be through multistage concentration, de-
The operations such as sulfur, decolouring produce 75% or 85% Wet Phosphoric Acid Market, but require relatively low for the phosphoric acid by wet process producing urea phosphate,
Only can be met to f with strip liquor-、so4 2-、al3+And fe3+Requirement Deng impurity；Additionally, adopting 75% or 85% wet cleaning phosphorus
Acid produces urea phosphate, and crystallization and mother liquor mixture solid-to-liquid ratio are larger, and mobility is bad, and separation of solid and liquid process are difficult.
Content of the invention
For solving above technical problem, it is an object of the invention to provide a kind of continuous, low cost, high income feed grade phosphorus
The production method of sour urea.
The object of the invention is realized in: a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce feed grade phosphorus
The method of sour urea comprises the following steps；
To in reactive tank, first add p2o5Concentration is 25～40% Wet Phosphoric Acid Market strip liquors or scrub raffinate, controls temperature to be 60
~ 85 DEG C, mixing speed is 100 ~ 200 r/min, is incubated 10 ~ 20 min, then presses phosphoric acid and urea mol ratio for 1: 1.0～1.2
Carbamide, stirring reaction 60～90 min is added in reactive tank；
Reactant liquor concentrates p under vacuum2o5Concentration, makes p2o5Concentration is that 48 ~ 55% formation concentrate reaction mass；
Concentrate after reaction mass is cooled to 5 ~ 40 DEG C and add crystal seed, cooling thermostatical crystallization separates out under 5 ~ 30 r/min stirring conditions
Urea phosphate；
Urea phosphate through centrifugation, be dried to obtain feed grade urea phosphate.
Preferably, in reactive tank, first add p2o5Concentration is 25～40% Wet Phosphoric Acid Market strip liquors or scrub raffinate, control
Temperature processed is 60 ~ 85 DEG C, and mixing speed is 100 ~ 150 r/min, is incubated 10 ~ 20 min, then presses phosphoric acid and urea mol ratio for 1
: 1.0～1.2 add carbamide, stirring reaction 70～90 min in reactive tank.
Preferably, reactant liquor evaporates p under -0.04 ~ -0.07mpa vacuum condition2o5Concentration is to 48 ~ 55%.
Preferably, concentrate reaction mass cooling crystallization process to be carried out in two steps in crystallization tank, one-level cools
In be cooled to 30 ~ 40 DEG C, be cooled to 5 ~ 30 DEG C in two grades of decrease temperature crystallines, during two grades of decrease temperature crystallines add crystal seed, constant temperature
Crystallization separates out urea phosphate, and crystallization temperature retention time is 2 ~ 5 h.
Preferably, the mixing speed during two grades of decrease temperature crystallines is 5 ~ 30r/min.
Preferably, the urea phosphate crystal through step with centrifugal separation is delivered to fluid bed, be dried extremely at a temperature of 50 ~ 70 DEG C
Material moisture≤1.5 % obtains feed grade urea phosphate.
Preferably, urea phosphate collects the recovered liquid separated in centrifugal separation processes；
Recovered liquid is delivered in the cooling groove that urea phosphate one-level cools.
Preferably, urea phosphate evaporation and concentration adopts circulating concentrated in vacuo, and negative pressure is atomized condenser or big by wet shotcrete technology
Gas condenser provides, and concentration material adopts punishment in advance to export.
The present invention provide a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate produce feed grade urea phosphate method, with
Compare advantage toward technology to be:
1) extracting and purifying phosphoric acid strip liquor or cleaning mixture continuously produce feed grade urea phosphate for raw material to this method in a wet process, it is to avoid
The impact that in phosphoric acid by wet process, foreign ion crystallizes to urea phosphate, for 75% or 85% finished product phosphoric acid, produces into meanwhile
This is lower；
2), in the cooling groove that recovered liquid circulation and stress to one-level cools, under the conditions of ensureing product purity, improve phosphorus
Sour urea ultimate yield, carries out self cooling cooling using the urea phosphate mother solution cold of itself to urea phosphate reactant liquor simultaneously, decreases and follow
Ring cooling water amount, reduces energy consumption；
3) activator or suspending agent etc. need not be added in production process, technological process is simple, has higher economic worth.
Brief description
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
Case study on implementation 1
As shown in Fig. 1, open stirring paddle, control rotating speed is 100 ~ 150r/min, add p in reactive tank2o5Concentration is
35% Wet Phosphoric Acid Market strip liquor, is passed through automatic steam control reaction temperature and is 70 DEG C, be incubated 10min；By carbamide and phosphoric acid mole
Add carbamide than for 1:1.0 ~ 1.1 in reactive tank, react 60 min；Reacted feed liquid is by being pumped into circulating vacuum
Concentrate in enrichment facility, control pressure is -0.05mpa, thickening temperature is 80 DEG C, and question response liquid is concentrated into p2o5After 50%, thing
Material is delivered to one-level crystallisation by cooling groove (one-level cools) by pump and is cooled to 40 DEG C, puts to two grades of cooling bath (two grades of coolings
Crystallization) it is cooled to 28 DEG C, the mixing speed during two grades of decrease temperature crystallines is 5 ~ 10r/min, adds crystal seed (2-5h) crystallization analysis
Go out urea phosphate；Through centrifugation, drying, baking temperature controls at 55 ~ 60 DEG C urea phosphate, obtains feed grade urea phosphate product,
p2o5Yield is 75.6%, n yield is 76%.
Case study on implementation 2
Carried out with the production method of embodiment 1 and technological parameter, difference is stated as follows, carbamide and phosphoric acid molar ratios are 1:
1.1 ~ 1.2, pressure concentrated in vacuo is -0.06mpa, concentrated solution p2o5Concentration be 52%；Crystal seed is added in two grades of decrease temperature crystallines
Temperature is 20 DEG C, and the mixing speed during two grades of decrease temperature crystallines is 20 ~ 30r/min, and urea phosphate is received in centrifugal separation processes
Collect the recovered liquid separated, recovered liquid is delivered in urea phosphate one-level crystallisation by cooling groove；In gained feed grade urea phosphate product
p2o5Yield is 85%, n yield is 85.5%.
Case study on implementation 3
As shown in Fig. 1, open stirring paddle, control rotating speed is 100 ~ 150r/min, add p in reactive tank2o5Concentration is
35% Wet Phosphoric Acid Market scrub raffinate, is passed through automatic steam control temperature and is 75 ~ 80 DEG C, be incubated 10 min, by carbamide and phosphoric acid mole
Add carbamide than for 1:1.0 ~ 1.05 in reactive tank, react 70 ~ 80 min；Reacted feed liquid is circulating by being pumped into
Concentrate in vacuum concentrating apparatus, control pressure is -0.05mpa, question response liquid is concentrated into p2o5After 50%, material is conveyed by pump
To one-level cooling bath, put after being cooled to 30 DEG C and continue to be cooled to 25 DEG C to two grades of crystallisation by cooling grooves, add seeded crystallization precipitation of phosphorus
Sour urea；Through centrifugation, drying, baking temperature controls at 55 ~ 60 DEG C urea phosphate, obtains feed grade urea phosphate product, p2o5
Yield is 75.0%, n yield is 75.2%.
Preferably, urea phosphate evaporation and concentration adopts circulating concentrated in vacuo, and negative pressure is atomized condenser or big by wet shotcrete technology
Gas condenser provides, and concentration material adopts punishment in advance to export.
Case study on implementation 4
As shown in Fig. 1, open stirring paddle, control rotating speed is 120 ~ 130r/min, add p in reactive tank2o5Concentration is
35% Wet Phosphoric Acid Market strip liquor, is passed through automatic steam control reaction temperature and is 70 DEG C, be incubated 10min；By carbamide and phosphoric acid mole
Add carbamide than for 1:1.0 ~ 1.1 in reactive tank, react 60 min；Reacted feed liquid is by being pumped into circulating vacuum
Concentrate in enrichment facility, control pressure is -0.05mpa, thickening temperature is 75 DEG C, and question response liquid is concentrated into p2o5After 50%, thing
Material is delivered to one-level crystallisation by cooling groove (one-level cools) by pump and is cooled to 40 DEG C, puts to two grades of cooling bath (two grades of coolings
Crystallization) it is cooled to 28 DEG C, the mixing speed during two grades of decrease temperature crystallines is 5 ~ 10r/min, adds crystal seed (2-5h) crystallization analysis
Go out urea phosphate；Through centrifugation, drying, baking temperature controls at 55 ~ 60 DEG C urea phosphate, obtains feed grade urea phosphate product,
p2o5Yield is 76.1%, n yield is 77%.
Claims (8)
1. a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce feed grade urea phosphate method it is characterised in that: institute
The method of stating comprises the following steps；
To in reactive tank, first add p2o5Concentration be 25～40% Wet Phosphoric Acid Market strip liquors or scrub raffinate, control temperature be 60 ~
85 DEG C, mixing speed is 100 ~ 200 r/min, is incubated 10 ~ 20 min, then press phosphoric acid and urea mol ratio for 1: 1.0～1.2 to
Carbamide, stirring reaction 60～90 min is added in reactive tank；
Reactant liquor concentrates p under vacuum2o5Concentration, makes p2o5Concentration is that 48 ~ 55% formation concentrate reaction mass；
Concentrate after reaction mass is cooled to 5 ~ 40 DEG C and add crystal seed, cooling thermostatical crystallization separates out under 5 ~ 30 r/min stirring conditions
Urea phosphate；
Urea phosphate through centrifugation, be dried to obtain feed grade urea phosphate.
2. according to claim 1, a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate produce the side of feed grade urea phosphate
Method it is characterised in that: in reactive tank, first add p2o5Concentration is 25～40% Wet Phosphoric Acid Market strip liquors or scrub raffinate, control
Temperature processed is 60 ~ 85 DEG C, and mixing speed is 100 ~ 150 r/min, is incubated 10 ~ 20 min, then presses phosphoric acid and urea mol ratio for 1
: 1.0～1.2 add carbamide, stirring reaction 70～90 min in reactive tank.
3. a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce feed grade urea phosphate according to claim 1
Method it is characterised in that: reactant liquor evaporates p under -0.04 ~ -0.07mpa vacuum condition2o5Concentration is to 48 ~ 55%.
4. a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce the side of feed grade urea phosphate according to claim 1
Method it is characterised in that: concentrate reaction mass cooling crystallization process be carried out in two steps in crystallization tank, during one-level cools
It is cooled to 30 ~ 40 DEG C, in two grades of decrease temperature crystallines, is cooled to 5 ~ 30 DEG C, add crystal seed during two grades of decrease temperature crystallines, constant temperature is tied
Partial crystallization goes out urea phosphate, and crystallization temperature retention time is 2 ~ 5 h.
5. a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce the side of feed grade urea phosphate according to claim 4
Method it is characterised in that: the mixing speed during described two grades of decrease temperature crystallines be 5 ~ 30r/min.
6. a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce feed grade urea phosphate according to claim 1
Method it is characterised in that: the urea phosphate crystal through step with centrifugal separation is delivered to fluid bed, at a temperature of 50 ~ 70 DEG C be dried
Obtain feed grade urea phosphate to material moisture≤1.5 %.
7. according to claim 1, a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce feed grade urea phosphate
Method it is characterised in that: described urea phosphate collects the recovered liquid separated in centrifugal separation processes；
Recovered liquid is delivered in the cooling groove that urea phosphate one-level cools.
8. a kind of Wet Phosphoric Acid Market strip liquor or scrub raffinate continuously produce feed grade urea phosphate according to claim 3
Method it is characterised in that: described urea phosphate evaporation and concentration adopt circulating concentrated in vacuo, negative pressure is atomized condenser by wet shotcrete technology
Or barometric condenser provides, concentration material adopts punishment in advance to export.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610721841.0A CN106349116A (en) | 2016-08-25 | 2016-08-25 | Method for continuously producing feed-grade urea phosphate from wet-method purified phosphoric acid strip liquor or washing residual liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162935A (en) * | 2017-05-27 | 2017-09-15 | 深圳市深投环保科技有限公司 | The recovery method of phosphorus-containing compound in useless chemical polishing agent |
| CN107188861A (en) * | 2017-05-27 | 2017-09-22 | 深圳市深投环保科技有限公司 | Recycle the method that phosphorous acid waste liquid prepares melamine polyphosphate |
| CN107473990A (en) * | 2017-07-24 | 2017-12-15 | 湖北三宁化工股份有限公司 | A kind of urea phosphate mother liquor water soluble fertilizer and preparation method |
| CN110452023A (en) * | 2019-08-08 | 2019-11-15 | 宜都兴发化工有限公司 | A kind of additive of complex fertilizer |
| CN110790683A (en) * | 2019-12-09 | 2020-02-14 | 武汉科技大学 | Method for producing urea phosphate by wet-process phosphoric acid elution coupling cooling 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107162935A (en) * | 2017-05-27 | 2017-09-15 | 深圳市深投环保科技有限公司 | The recovery method of phosphorus-containing compound in useless chemical polishing agent |
| CN107188861A (en) * | 2017-05-27 | 2017-09-22 | 深圳市深投环保科技有限公司 | Recycle the method that phosphorous acid waste liquid prepares melamine polyphosphate |
| CN107162935B (en) * | 2017-05-27 | 2019-05-24 | 深圳市深投环保科技有限公司 | The recovery method of phosphorus-containing compound in useless chemical polishing agent |
| CN107188861B (en) * | 2017-05-27 | 2020-05-08 | 深圳市深投环保科技有限公司 | Method for preparing melamine polyphosphate by recycling phosphorus-containing acidic waste liquid |
| CN107473990A (en) * | 2017-07-24 | 2017-12-15 | 湖北三宁化工股份有限公司 | A kind of urea phosphate mother liquor water soluble fertilizer and preparation method |
| CN110452023A (en) * | 2019-08-08 | 2019-11-15 | 宜都兴发化工有限公司 | A kind of additive of complex fertilizer |
| CN110790683A (en) * | 2019-12-09 | 2020-02-14 | 武汉科技大学 | Method for producing urea phosphate by wet-process phosphoric acid elution coupling cooling 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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Application publication date: 20170125 |