CN107033034A - A kind of production technology of urea phosphate - Google Patents
A kind of production technology of urea phosphate Download PDFInfo
- Publication number
- CN107033034A CN107033034A CN201710423006.3A CN201710423006A CN107033034A CN 107033034 A CN107033034 A CN 107033034A CN 201710423006 A CN201710423006 A CN 201710423006A CN 107033034 A CN107033034 A CN 107033034A
- Authority
- CN
- China
- Prior art keywords
- phosphoric acid
- solution
- urea phosphate
- urea
- slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
Abstract
The present invention discloses a kind of production technology of urea phosphate, comprises the following steps：1) phosphoric acid solution is pre-processed：Alkaline conditioner and acid regulator, mixed dissolution are added into phosphoric acid solution successively, mixed solution A is obtained；Wherein, the concentration of phosphoric acid solution is with P2O5It is calculated as 25 35wt%；2) preparation of slurry：1 2h is reacted by obtained mixed solution A and urea mixed dissolution, and at 70 80 DEG C, slurry is obtained；3) crystallisation by cooling：Obtained slurry is carried out after being once evaporated in vacuo, a crystallisation by cooling is carried out at 40 50 DEG C, filtered to get filtrate B and crystallization, and gained is crystallized into washing and drying, urea phosphate is obtained；4) secondary cooling is crystallized：By step 3) in gained liquor B carry out secondary vacuum evaporation after, at 20 30 DEG C carry out secondary cooling crystallization, separate supernatant mother solution C, it can be used as fertilizer, lower floor's magma and step 2) in gained slurry mix, and press step 3) operate.
Description
Technical field
The present invention relates to technical field of fine, and in particular to a kind of production technology of urea phosphate.
Background technology
Urea phosphate is also known as urea phosphoric acid or urea phosphate, is a kind of coordination by equimolar phosphoric acid and urea reaction generation
Compound.Early in 1914, BASF Aktiengesellschaft just applied for preparing the patent of urea phosphate, but until urea is realized on a large scale
After production and cost are significantly reduced, urea phosphate just really becomes industrial products and is widely used in animal husbandry and industrial and agricultural production
In.At present, the application of urea phosphate is non-by being mainly used as efficient nitrogen, phosphorus composite fertilizer and the ruminant of animal husbandry and agricultural originally
Proteinic nitrogen (NPN) feed addictive, gradually develops to field of industrial production, is such as used as metal cleaner, fire retardant, high temperature resistant and glues
The multiple fields such as mixture, fabric finishing agent.
The production method of urea phosphate, can be divided into wet phosphoric acid, thermal phosphoric acid method and polymer phosphate method by raw material sources.Heat
Method phosphoric acid concentration is high, and phosphoric acid price is costly, higher to produce urea phosphate cost；Polymer phosphate method is limited by raw material sources,
It is rarely used；Phosphoric acid by wet process concentration is relatively low, and impurity is more, but the cost of phosphoric acid is relatively low, low to produce urea phosphate cost.Mesh
Before, the technique of Wet-process phosphoric acid (WPPA) urea is optimized the Chinese patent of Application No. 200810068832.1, it discloses
A kind of method that urea phosphate is produced by raw material of phosphoric acid by wet process, this method adds reacting movable agent and suspension during the course of the reaction
Agent, promotes the progress of reaction, but also increases reaction cost, simultaneously because the impurity in phosphoric acid is not removed, so as to cause
Urea phosphate phosphrus reagent is relatively low.
The content of the invention
In view of this, the application provides a kind of production technology of urea phosphate, low excellent with urea phosphate phosphrus reagent height, cost
Point.
To solve above technical problem, the technical scheme that the present invention is provided is a kind of production technology of urea phosphate, and it includes
Following steps：
1) phosphoric acid solution is pre-processed：Alkaline conditioner and acid regulator are added into phosphoric acid solution successively, is mixed molten
Solution, obtains mixed solution A；Wherein, the concentration of phosphoric acid solution is with P2O5It is calculated as 25-35wt%；
2) preparation of slurry：1-2h is reacted by obtained mixed solution A and urea mixed dissolution, and at 70-80 DEG C, is obtained
To slurry；
3) crystallisation by cooling：Obtained slurry is carried out after being once evaporated in vacuo, once cooled down at 40-50 DEG C
Crystallization, filtered to get filtrate B and crystallization, and gained is crystallized into washing and drying, urea phosphate is obtained；
4) secondary cooling is crystallized：By step 3) in gained liquor B carry out secondary vacuum evaporation after, at 20-30 DEG C carry out
Secondary cooling is crystallized, and separates supernatant mother solution C, it can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step
It is rapid 3) to operate.
It is preferred that, step 1) described in mixed solution A be made by following methods：Alkalescence regulation is added into phosphoric acid solution
Agent, mixed dissolution filters waste discharge, obtains single treatment phosphoric acid solution；Acid regulator is added into single treatment phosphoric acid solution, is mixed
Dissolving is closed, after-treatment phosphoric acid solution, i.e. mixed solution A is obtained.
It is preferred that, the mass ratio for adding phosphoric acid solution, alkaline conditioner and acid regulator is (1-1.5)：
(0.8-1.2)：(1.5-2).
It is preferred that, the mass ratio for adding phosphoric acid solution, alkaline conditioner and acid regulator is (1-1.2)：
(0.8-1)：(1.8-2).
It is preferred that, the alkaline conditioner is the one or more in sodium hydroxide, sodium acid carbonate or disodium hydrogen phosphate；Acid
Property conditioning agent be citric acid, dilute sulfuric acid, watery hydrochloric acid or phosphoric acid in one or more.
It is preferred that, the alkaline conditioner is sodium hydroxide；Acid regulator is dilute sulfuric acid.
It is preferred that, it is 30-45wt% that hydrionic concentration in acid regulator is added in the phosphoric acid solution.
It is preferred that, it is 30-40wt% that hydrionic concentration in acid regulator is added in the phosphoric acid solution.
It is preferred that, the concentration of the phosphoric acid solution is with P2O5It is calculated as 25-30wt%.
It is preferred that, step 2) described in mixed solution A and urea mass ratio be 1：(0.5-1.5).
It is preferred that, the mass ratio of the mixed solution A and urea is 1：(0.8-1).
It is preferred that, step 3) described in a crystallisation by cooling comprise the following steps that：By obtained slurry 0.5-0.8Mpa,
A vacuum evaporation is carried out at 70-75 DEG C, after the completion of vacuum evaporation, crystallisation by cooling of progress at 45-50 DEG C, and with
5000rpm centrifugal speed is filtered, and filtered to get filtrate B and crystallization, and gained is crystallized into washing and drying, urea phosphate is obtained.
It is preferred that, step 4) described in secondary cooling crystallization comprise the following steps that：By step 3) in gained liquor B in 1.0-
1.3Mpa, secondary vacuum evaporation and concentration is carried out at 75-80 DEG C, after the completion of vacuum evaporation, secondary cooling knot is carried out at 20-25 DEG C
Crystalline substance, and separated with 5000rpm centrifugal speed, supernatant mother solution C and lower floor's magma are obtained, supernatant mother solution C can be used as fertilizer, under
Layer magma and step 2) middle gained slurry is mixed, and press step 3) operation.
The present invention provides a kind of production technology of urea phosphate, and it includes pre-processing phosphoric acid solution, the preparation of slurry, once cold
But crystallization and secondary cooling crystallize four steps.First, alkaline conditioner is used in the application for sodium hydroxide, using hydroxide
Sodium is pre-processed to phosphoric acid, the reason is that wet phosphoric acid prepares urea phosphate, although its production cost is relatively low, its institute
Relatively low with the content of raw material phosphor, impurity content is high, and the content of fluorine is higher in impurity, and the main presence in the form of fluosilicic acid, leads to
Cross research to show, the presence of fluorine ion can reduce the yield of phosphorus in urea phosphate in phosphoric acid, therefore use sodium hydroxide in the application
Phosphoric acid is pre-processed, it is richer than the prodan of water with fluosilicic acid reaction generation hardly possible, so that fluorine impurity be removed.Meanwhile,
In the application also to pretreated phosphoric acid carry out after-treatment, the reason is that in acid regulator containing substantial amounts of hydrogen from
Son, its can hydrionic concentration in increase system, promote the progress of reaction, promote the precipitation of urea phosphate crystal, improve the receipts of phosphorus
Rate, so as to reduce production cost.
Secondly, second-crystallized method is used in the application, the reason is that reaction slurry is through being once evaporated in vacuo, crystallizing
Still there is a small amount of phosphoric acid and impurity after filter, in its mother liquor, therefore, the mother liquor after filtering is subjected to secondary vacuum evaporation and gone forward side by side
Row reducing temperature twice crystallization filtering, supernatant mother liquor can be as Fertilizer application, and lower floor's magma is mixed with the slurry in reactor carries out the
Secondary dissolving, by being further evaporated in vacuo, crystallizing after filtering, improves the eduction rate of urea phosphate, so that the yield of phosphorus is improved,
Reduce production cost.
Finally, the step of adding vacuum evaporation before crystallization process in the application, the reason is that being adopted in the application
Raw material is with P2O525-35wt% phosphoric acid solution is calculated as, the content of its phosphorus is relatively low, is found by studying, in production
During ureasulfuric acid, using 40%P2O5Phosphoric acid above can just produce crystallization.Therefore, in primary crystallization and two in the application
It is respectively adopted and is once evaporated in vacuo and secondary vacuum evaporation before secondary crystallization, so that P2O5Content meet crystallization needed for.
A kind of production technology of urea phosphate specifically preferred according to the invention, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Dilute sulfuric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 35% wherein, to add phosphoric acid solution, hydrogen in dilution heat of sulfuric acid
The mass ratio of sodium oxide molybdena and dilute sulfuric acid is 1：0.8：1.5；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 93%.
The positive achievement that the present invention is obtained is：
1st, the present invention carries out alkali process and acid treatment respectively to the phosphoric acid before reaction, wherein, sodium hydroxide can be with fluosilicic acid
Reaction, removes the fluorine impurity in phosphoric acid, the eduction rate of urea phosphate is improved, so as to improve phosphrus reagent in urea phosphate；Acid is carried out to it
Processing, can hydrionic concentration in increase system, promote the precipitation of urea phosphate crystal, improve the yield of phosphorus, reduce and be produced into
This.
2nd, the present invention produces urea phosphate using second-crystallized method, the eduction rate of urea phosphate can be improved, so as to improve the receipts of phosphorus
Rate, reduces production cost.
3rd, the step of present invention adds vacuum evaporation before crystallization process, so that P2O5Content meet crystallization needed for.
Brief description of the drawings
Fig. 1 is process chart of the invention
Embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to specific embodiment pair
The present invention is described in further detail.
Urea phosphate is also known as urea phosphate.Chemical fertilizer industry is developed rapidly since with 1960s, to urea phosphate
Structure, property, the research of preparation technology receive attention, the application field of urea phosphate also constantly expands.Nitrogen phosphorus in urea phosphate
Total nutrient is up to 63%, after hydrolysis of burying, and the acidity of generation reduces the pH value of soil, is particularly suitable for use in basic soil, can be big
The big volatilization loss for reducing ammonia, therefore the product is a kind of very capable high-efficiency compound fertilizer of guarantor's nitrogen.Ureasulfuric acid also can with nitre ammonia,
Multi-elements composite fertilizer of the mixing composition such as calcareous fertilisers, potash fertilizer, trace element containing nutritional ingredient up to 70%.Liquid based on urea phosphate
State fertilizer can be sprayed together with herbicide, insecticide.
Urea phosphate is, using urea and phosphoric acid as base stock, to react obtained under certain condition, reaction equation is：
H3PO4+CO(NH2)2=CO (NH2)2·H3PO4
At present, the production technology of urea phosphate press raw materials used phosphoric acid difference, be divided into thermal phosphoric acid method, wet phosphoric acid and
Polymer phosphate method.Wherein, thermal phosphoric acid method synthesis urea phosphate refers to technique thermal phosphoric acid (containing amount≤85%) and agricultural urea
(Han Liang≤46%) press in metered reactor, crystallize, separation, dry obtained product.Product yield is reachable after it reacts
More than 98%, and feed grade ureasulfuric acid can be directly obtained, but its major defect is, the cost of raw material is higher.Phosphoric acid by wet process is closed
Into urea phosphate, its production cost is low, but its raw materials used phosphorus content is low, and impurity content is high, hardly result in ureasulfuric acid phosphrus reagent compared with
High product.And polymer phosphate method is limited larger by raw material sources, therefore it is rarely used.
In the application, raw materials used is with P2O5Be calculated as 25-35wt% phosphoric acid solution, its phosphorus content is relatively low, fluorinated volume compared with
Height, fluorine exists typically in the form of fluosilicic acid, and phosphoric acid is pre-processed using sodium hydroxide, and it can pass through fluosilicic acid and hydrogen-oxygen
Change sodium reaction, generation prodan precipitation removes impurity fluorine, and its reaction equation is as follows：
H2SiF6+ 2NaOH=Na2SiF6↓+2H2O
Meanwhile, the application carries out after-treatment to the phosphoric acid after naoh treatment, and it is by adding in acid, increase system
Hydrogen ion so that promote reaction progress, promote ureasulfuric acid generation, improve urea phosphate phosphorus yield.
The technical scheme that the present invention is provided is a kind of production technology of urea phosphate, is comprised the following steps：
1) phosphoric acid solution is pre-processed：Alkaline conditioner and acid regulator are added into phosphoric acid solution successively, is mixed molten
Solution, obtains mixed solution A；Wherein, the concentration of phosphoric acid solution is calculated as 25-35wt% with P2O5；
2) preparation of slurry：1-2h is reacted by obtained mixed solution A and urea mixed dissolution, and at 70-80 DEG C, is obtained
To slurry；
3) crystallisation by cooling：Obtained slurry is carried out after being once evaporated in vacuo, once cooled down at 40-50 DEG C
Crystallization, filtered to get filtrate B and crystallization, and gained is crystallized into washing and drying, urea phosphate is obtained；
4) secondary cooling is crystallized：By step 3) in gained liquor B carry out secondary vacuum evaporation after, at 20-30 DEG C carry out
Secondary cooling is crystallized, and separates supernatant mother solution C, it can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step
It is rapid 3) to operate.
Wherein, step 1) described in mixed solution A be made by following methods：Alkaline conditioner is added into phosphoric acid solution,
Mixed dissolution, filters waste discharge, obtains single treatment phosphoric acid solution；Acid regulator is added into single treatment phosphoric acid solution, is mixed
Dissolving, obtains after-treatment phosphoric acid solution, i.e. mixed solution A.Wherein, the addition phosphoric acid solution, alkaline conditioner and acidity
The mass ratio of conditioning agent is (1-1.5)：(0.8-1.2)：(1.5-2)；It is preferred that, the addition phosphoric acid solution, alkaline conditioner
And the mass ratio of acid regulator is (1-1.2)：(0.8-1)：(1.8-2).Wherein, the alkaline conditioner is hydroxide
One or more in sodium, sodium acid carbonate or disodium hydrogen phosphate；Acid regulator is citric acid, dilute sulfuric acid, watery hydrochloric acid or phosphoric acid
In one or more.Wherein, it is 30-45wt% that hydrionic concentration in acid regulator is added in the phosphoric acid solution.；It is excellent
Choosing, it is 30-45wt% that hydrionic concentration in acid regulator is added in the phosphoric acid solution..
Wherein, step 2) described in mixed solution A and urea mass ratio be 1：(0.5-1.5)；It is preferred that, the mixing
The mass ratio of solution A and urea is 1：(0.8-1).Wherein, step 3) described in a crystallisation by cooling comprise the following steps that：Will
The slurry arrived carries out a vacuum evaporation at 0.5-0.8Mpa, 70-75 DEG C, after the completion of vacuum evaporation, at 45-50 DEG C
A crystallisation by cooling is carried out, and is filtered with 5000rpm centrifugal speed, filter to get filtrate B and crystallization, by the gained crystallization water
Drying is washed, urea phosphate is obtained.Wherein, step 4) described in secondary cooling crystallization comprise the following steps that：By step 3) middle gained liquor B
Secondary vacuum evaporation and concentration is carried out at 1.0-1.3Mpa, 75-80 DEG C, after the completion of vacuum evaporation, is carried out at 20-25 DEG C secondary
Crystallisation by cooling, and separated with 5000rpm centrifugal speed, supernatant mother solution C and lower floor's magma are obtained, supernatant mother solution C can be used as
Fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
The commercially available gained of reagent and raw material used in the present invention.
Below in conjunction with embodiments of the invention, technical scheme is clearly and completely described, it is clear that
Described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made is belonged to
The scope of protection of the invention.
Embodiment one：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding dilute sulfuric acid, mixed dissolution mixes
Close solution A；Wherein, hydrionic concentration is the quality for 35% wherein adding phosphoric acid solution and dilute sulfuric acid in dilution heat of sulfuric acid
Than for 1：1.5；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 82%.
Embodiment two：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Filter waste discharge, the phosphoric acid solution after must handling, i.e. mixed solution A；Wherein, add phosphoric acid solution and the mass ratio of sodium hydroxide is
1：0.8；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 79%.
Embodiment three：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium acid carbonate, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Watery hydrochloric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 35% wherein, to add phosphoric acid solution, carbon in dilute hydrochloric acid solution
The mass ratio of sour hydrogen sodium and watery hydrochloric acid is 1：0.8：1.5；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 91%.
Example IV：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Dilute sulfuric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 35% wherein, to add phosphoric acid solution, hydrogen in dilution heat of sulfuric acid
The mass ratio of sodium oxide molybdena and dilute sulfuric acid is 1：0.8：1.5；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 93%.
Embodiment five：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 30wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Dilute sulfuric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 30% wherein, to add phosphoric acid solution, hydrogen in dilution heat of sulfuric acid
The mass ratio of sodium oxide molybdena and dilute sulfuric acid is 1：1.2：2；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 85%.
Embodiment six：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Dilute sulfuric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 35% wherein, to add phosphoric acid solution, hydrogen in dilution heat of sulfuric acid
The mass ratio of sodium oxide molybdena and dilute sulfuric acid is 1：0.8：1.5；
2) preparation of slurry：1.5h is reacted by obtained mixed solution A and urea mixed dissolution, and at 80 DEG C, is obtained
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：0.8；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 90%.
Embodiment seven：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Dilute sulfuric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 35% wherein, to add phosphoric acid solution, hydrogen in dilution heat of sulfuric acid
The mass ratio of sodium oxide molybdena and dilute sulfuric acid is 1：0.8：1.5；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.6Mpa, 73 DEG C, after the completion of vacuum evaporation, 50
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.0Mpa, 80 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 20 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 87%.
Embodiment eight：
A kind of production technology of urea phosphate, comprises the following steps：
1) phosphoric acid solution is pre-processed：To with P2O5It is calculated as in 25wt% phosphoric acid solutions adding sodium hydroxide, mixed dissolution, mistake
Waste discharge is filtered, single treatment phosphoric acid solution is obtained；Dilute sulfuric acid is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment
Phosphoric acid solution, i.e. mixed solution A；Wherein, hydrionic concentration is 35% wherein, to add phosphoric acid solution, hydrogen in dilution heat of sulfuric acid
The mass ratio of sodium oxide molybdena and dilute sulfuric acid is 1：0.8：1.5；
2) preparation of slurry：1h is reacted by obtained mixed solution A and urea mixed dissolution, and at 75 DEG C, is expected
Slurry；Wherein, the mass ratio of mixed solution A and urea is 1：1；
3) obtained slurry is subjected to a vacuum evaporation at 0.8Mpa, 70 DEG C, after the completion of vacuum evaporation, 45
A crystallisation by cooling is carried out at DEG C, and is filtered with 5000rpm centrifugal speed, filtered to get filtrate B and crystallization, and gained is tied
Brilliant washing and drying, obtains urea phosphate.
4) by step 3) in gained liquor B carries out secondary vacuum evaporation and concentration at 1.3Mpa, 75 DEG C, be evaporated in vacuo completion
Afterwards, secondary cooling crystallization is carried out at 23 DEG C, and is separated with 5000rpm centrifugal speed, supernatant mother solution C is obtained and lower floor is thick
Liquid, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3) operation.
Through examining, obtained urea phosphate is produced according to above-mentioned production technology, its phosphrus reagent is 82%.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of production technology of urea phosphate, it is characterised in that comprise the following steps：
1) phosphoric acid solution is pre-processed：Alkaline conditioner and acid regulator, mixed dissolution are added into phosphoric acid solution successively, is obtained
To mixed solution A；Wherein, the concentration of phosphoric acid solution is with P2O5It is calculated as 25-35wt%；
2) preparation of slurry：1-2h is reacted by obtained mixed solution A and urea mixed dissolution, and at 70-80 DEG C, is expected
Slurry；
3) crystallisation by cooling：Obtained slurry is carried out after being once evaporated in vacuo, knot is once cooled down at 40-50 DEG C
Crystalline substance, filtered to get filtrate B and crystallization, and gained is crystallized into washing and drying, urea phosphate is obtained；
4) secondary cooling is crystallized：By step 3) in gained liquor B carry out secondary vacuum evaporation after, carried out at 20-30 DEG C secondary
Crystallisation by cooling, separates supernatant mother solution C, it can be used as fertilizer, lower floor's magma and step 2) middle gained slurry is mixed, and press step 3)
Operation.
2. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 1) described in mixed solution
A is made by following methods：Alkaline conditioner is added into phosphoric acid solution, mixed dissolution filters waste discharge, obtains single treatment phosphoric acid molten
Liquid；Acid regulator is added into single treatment phosphoric acid solution, mixed dissolution obtains after-treatment phosphoric acid solution, i.e. mixed solution
A。
3. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 1) described in add phosphoric acid
The mass ratio of solution, alkaline conditioner and acid regulator is (1-1.5)：(0.8-1.2)：(1.5-2).
4. a kind of production technology of urea phosphate according to claim 1, it is characterised in that the alkaline conditioner is hydrogen-oxygen
Change the one or more in sodium, sodium acid carbonate or disodium hydrogen phosphate；Acid regulator is citric acid, dilute sulfuric acid, watery hydrochloric acid or phosphorus
One or more in acid.
5. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 1) described in phosphoric acid solution
Hydrionic concentration is 30-45wt% in middle addition acid regulator.
6. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 1) phosphoric acid solution
Concentration is with P2O5It is calculated as 25-30wt%.
7. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 2) described in mixed solution
The mass ratio of A and urea is 1：(0.5-1.5).
8. a kind of production technology of urea phosphate according to claim 7, it is characterised in that the mixed solution A and urea
Mass ratio be 1：(0.8-1).
9. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 3) described in once cool down
Crystallization is comprised the following steps that：Obtained slurry is subjected to a vacuum evaporation, vacuum at 0.5-0.8Mpa, 70-75 DEG C
After the completion of evaporation, a crystallisation by cooling is carried out at 45-50 DEG C, and is filtered with 5000rpm centrifugal speed, filtering to filter
Liquid B and crystallization, washing and drying is crystallized by gained, obtains urea phosphate.
10. a kind of production technology of urea phosphate according to claim 1, it is characterised in that step 4) described in it is secondary cold
But crystallization is comprised the following steps that：By step 3) in gained liquor B secondary vacuum evaporation is carried out at 1.0-1.3Mpa, 75-80 DEG C
Concentration, after the completion of vacuum evaporation, carries out secondary cooling crystallization, and divided with 5000rpm centrifugal speed at 20-25 DEG C
From obtaining supernatant mother solution C and lower floor's magma, supernatant mother solution C can be used as fertilizer, lower floor's magma and step 2) in gained slurry mix,
And by step 3) operation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710423006.3A CN107033034A (en) | 2017-06-07 | 2017-06-07 | A kind of production technology of urea phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710423006.3A CN107033034A (en) | 2017-06-07 | 2017-06-07 | A kind of production technology of urea phosphate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107033034A true CN107033034A (en) | 2017-08-11 |
Family
ID=59541840
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710423006.3A Pending CN107033034A (en) | 2017-06-07 | 2017-06-07 | A kind of production technology of urea phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107033034A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111689875A (en) * | 2020-07-07 | 2020-09-22 | 中化云龙有限公司 | Method for producing feed-grade urea phosphate by using wet-process phosphoric acid residues |
Citations (1)
| 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 |
-
2017
- 2017-06-07 CN CN201710423006.3A patent/CN107033034A/en active Pending
Patent Citations (1)
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| 傅亚男等: "湿法磷酸的脱氟研究", 《贵州工业大学学报（自然科学版）》 * |
| 李云生: "湿法磷酸制备磷酸脲的试验研究", 《硫酸设计与粉体工程》 * |
| 谢萍: "磷酸脲生产工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 钟本和等: "湿法磷酸脱色脱氟实验研究", 《化肥工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111689875A (en) * | 2020-07-07 | 2020-09-22 | 中化云龙有限公司 | Method for producing feed-grade urea phosphate by using wet-process phosphoric acid residues |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105236448B (en) | A kind of new technology for producing coproduction of potassium sulfate composite fertilizer | |
| CN104211485B (en) | The method for producing crystalloid potassium dihydrogen phosphate and potassium nitrate a great number of elements Water soluble fertilizer | |
| CN106315625A (en) | Method for composite production of high-purity lithium hydroxide monohydrate, high-purity lithium carbonate and battery grade lithium carbonate | |
| CN113460989B (en) | Battery-grade iron phosphate and preparation method thereof | |
| CN106745156B (en) | A kind of method of decomposing phosphorite by using nitric acid coproduction potassium nitrate and nitric acid phosphorus potassium complex fertilizer | |
| CN107879363A (en) | A kind of method that nitric acid decomposes phosphorus mine tailing extracting sulfuric acid calcium pyroborate by-product magnesium hydroxide and ammonium nitrate magnesium | |
| CN106379918B (en) | A kind of method of acyclic preparing potassium nitrate by means of double decomposition combined producting ammonium chloride potassium | |
| CN105294469B (en) | A kind of preparation method of sodium iron ethylene diamine tetra acetate | |
| CN108183276A (en) | The preparation method of ferric phosphate | |
| CN106830021A (en) | A kind of preparation technology of magnesium nitrate hexahydrate | |
| CA1166425A (en) | Method of manufacturing potassium sulfate | |
| CN113526480A (en) | Method for preparing ferrous phosphate from titanium dioxide byproduct | |
| CN1736870A (en) | Method for preparing potassium nitrate using nitric acid conversion methdo | |
| CN107033034A (en) | A kind of production technology of urea phosphate | |
| CN105480959A (en) | Method for producing monopotassium phosphate by fluoride salt purification process | |
| CN1765746A (en) | Method for making potassium nitrate using magnesium hydroxide circular reaction method | |
| CN107792840A (en) | A kind of method that accessory substance ferrophosphorus using industrial yellow phosphorus production prepares ferric phosphate | |
| US3712942A (en) | Method of producing vanadium compounds by alkaline leaching | |
| CN103466583A (en) | Method of preparing iron phosphate by using phosphor-iron oxidizing slag | |
| CN111252750A (en) | Method for preparing iron phosphate and aluminum oxide from phosphorus aluminum slag | |
| CN104725281A (en) | Method for producing urea peroxide | |
| CN1034067C (en) | Preparation of potassium sulfate by circulating double decomposition of ammonium sulfate and potassium chloride | |
| CN111517832B (en) | Separation method of P, Ca in medium-low grade phosphate ore and method for producing fertilizer | |
| CN108117054A (en) | A kind of method for preparing potassium dihydrogen phosphate coproduction ammonium potassium dihydrogen phosphate | |
| CN107162022A (en) | Production of Potassium Nitrate method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170811 |