GB2077711A - Preparation of ammonium polyphosphate - Google Patents
Preparation of ammonium polyphosphate Download PDFInfo
- Publication number
- GB2077711A GB2077711A GB8116676A GB8116676A GB2077711A GB 2077711 A GB2077711 A GB 2077711A GB 8116676 A GB8116676 A GB 8116676A GB 8116676 A GB8116676 A GB 8116676A GB 2077711 A GB2077711 A GB 2077711A
- Authority
- GB
- United Kingdom
- Prior art keywords
- acid
- reactor
- process according
- ammonia
- chamber
- 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.)
- Granted
Links
- 235000019826 ammonium polyphosphate Nutrition 0.000 title claims abstract description 9
- 229920001276 ammonium polyphosphate Polymers 0.000 title claims abstract description 9
- 239000004114 Ammonium polyphosphate Substances 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 66
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims description 25
- 239000002253 acid Substances 0.000 claims description 24
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 19
- 229910052698 phosphorus Inorganic materials 0.000 claims description 19
- 239000011574 phosphorus Substances 0.000 claims description 19
- 235000011007 phosphoric acid Nutrition 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 239000001117 sulphuric acid Substances 0.000 claims description 3
- 235000011149 sulphuric acid Nutrition 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 9
- 239000007788 liquid Substances 0.000 abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 229920000388 Polyphosphate Polymers 0.000 description 9
- 239000001205 polyphosphate Substances 0.000 description 9
- 235000011176 polyphosphates Nutrition 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 4
- 235000011180 diphosphates Nutrition 0.000 description 4
- 239000003337 fertilizer Substances 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 235000019832 sodium triphosphate Nutrition 0.000 description 4
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 1
- MDLLTLUNXNWIIQ-UHFFFAOYSA-K azanium iron(3+) phosphonato phosphate Chemical compound [NH4+].[Fe+3].[O-]P([O-])(=O)OP([O-])([O-])=O MDLLTLUNXNWIIQ-UHFFFAOYSA-K 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000033001 locomotion Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B1/00—Superphosphates, i.e. fertilisers produced by reacting rock or bone phosphates with sulfuric or phosphoric acid in such amounts and concentrations as to yield solid products directly
- C05B1/06—Ammoniation of superphosphates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
- C01B25/405—Polyphosphates of ammonium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00105—Controlling the temperature by indirect heating or cooling employing heat exchange fluids part or all of the reactants being heated or cooled outside the reactor while recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Fertilizers (AREA)
Abstract
For preparing ammonium polyphosphate from gaseous ammonia and phosphoric acid, there is used a columnar reactor having a small cylindrical chamber (1), a bottleneck section (4), and a second cylindrical chamber (6) which is terminated by a discharge nozzle (7), a substantial portion of the reactor extending into a liquid bath (8). Part of the ammonia is fed to the reactor either to the top of the column via a bore (2) or laterally thereof via a bore (3) depending upon whether the ammonia is introduced simultaneously with the phosphoric acid or separately therefrom, and the remainder of the ammonia is fed to the reactor via a bore (5). Pressures of from 1.3 to 6 atmospheres are specified and temperatures in the neighbourhood of 300 DEG C are preferred. <IMAGE>
Description
SPECIFICATION
Preparation of ammonium polyphosphate
This invention relates to the preparation of ammonium polyphosphate which, when solubilised, can be used in the preparation of liquid fertilizers.
The term ammonium polyphosphate" used herein generally denotes a mixture of ammonium salts of orthophosphoric acid and of polyphosphoric acids.
In the last decade in particular, many processes for producing ammonium polyphosphates from phosphoric acid and ammonia have been suggested. However, they have a number of disadvantages. Some of these methods result in a low conversion of the phosphoric acid to the polycondensed form necessary for obtaining concentrated solutions which are free from precipitates for a long time. In other methods, phosphoric acid is processed in a plurality of stages requiring the use of bulky and intricate apparatus. In nearly all of the methods, the formation, in the primary stage of the reaction, of iron ammonium pyrophosphate is unavoidable. This compound is insoluble and forms incrustations of the apparatus, so that it is necessary to discontinue the reaction to effect cleaning.
According to the present invention, there is provided a process for the preparation of ammonium polyphosphate, which comprises reacting gaseous ammonia with an acid of phosphorus selected from orthophosphoric acid and/or superphosphoric acid in a vertical elongate reactor having a restricted section dividing the reactor into an upper restricted chamber and a lower elongate tubular chamber, the pressure in the reactor being from 1.3 to 6 atmospheres.
The present invention also provides an apparatus for use in carrying out a process according to the invention, comprising a vertical elongate reactor having a restricted section dividing the reactor into an upper restricted chamber and a lower elongate tubular chamber, the lower chamber being terminated by another restricted section.
The process according to this invention gives an end product which is normally stable with time, and which can be mixed with pesticides, fungicides and liquid fertilizers of the Uran type in all proportions.
In the process according to the present invention, gaseous ammonia is reacted with an acid of phosphorus selected from orthophosphoric acid and superphosphoric acid. When orthophosphoric acid is used, it is possible to add sulphuric acid thereto in an amount of up to 15% by weight relative to the orthophosphoric acid. Whether orthophosphoric or superphosphoric acid or both is used depends upon the conversion into the condensed forms one desires to prepare.
With superphosphoric acid, it is usually possible to attain a conversion of more than 80% into condensed form.
The acid of phosphorus, e.g. the orthophosphoric acid, may be an acid formed by a wet treatment, which acid does not necessarily require any preliminary purification prior to being used in the process of the invention. The acid of phosphorus, e.g. the orthophosphoric acid, used according to this invention usually has a content of P205 of from 56% to 62% by weight.
The pressure throughout the reactor is preferably substantially constant, and is from 1.3 to 6 atmospheres.
The reactants are preferably caused to contact one another in the most intimate manner possible and with intense whirling motions, so that molecule contacts are as many as possible.
This makes it possible to evolve all of the reaction heat, which is utilized to polycondense the acid of phosphorus. The melt obtained in the reaction may be discharged, diluted with water and allowed to cool to obtain a a liquid fertilizer having an appropriate concentration so as to obtain, for example, formulations of the kinds 11-30-0, 10-34-0 and 1 1-37-0.
According to a preferred embodiment of the invention, part of the ammonia is fed to the upper chamber (e.g. 60-80% of the total ammonia) either in admixture with the acid of phosphorus or separately therefrom, and the remainder of the ammonia is fed to the lower chamber, preferably near to the restricted section. The acid of phosphorus is usually fed to the top, or near to the top, of the upper chamber.
The apparatus which provides the best reaction conditions is generally comprised of a small chamber, preferably cylindrical, with the cylinder axis vertical, but can also be of any other possible form The chamber is terminated at the bottom in a gradual manner by a restricted section and is subsequently radiussed to a vertical tubular elongate chamber which, in its turn, is terminated by a "bottleneck" section. This narrowed section can be formed in various ways, such as, for example, by a nozzle, by a small plate, or by a fixed or movable cone, and is intended to maintain the desired pressure within the entire apparatus.
The restricted section at the bottom of the cylindrical chamber is usually from 20 to 30% wider than the narrowed section which closes the elongate tubular vertical chamber. The latter chamber, along a consistent length thereof, may extend into a vessel which is open at its top and may have any desired shape, and which may contain a preformed liquid appropriate to the fertilizer to be prepared and to which water only is added to attain the desired concentration.
This vessel usually collects all of the liquid and gaseous fluids exiting the reactor, and its contents, appropriately mixed may be subjected to recycling for cooling at a temperature of, for example 40 to 60"C. Preferably, the acid of phosphrous, preheated to a temperature of from 100 to 1 35"C, is fed to the top or near to the top of the small cylindrical chamber in a finely atomised state. This can be achieved in a number of ways, such as, for example, by use of a spraying nozzle.
According to a preferred embodiment of the invention, the acid of phosphorus is atomized, at the top of the cylindrical chamber, with a quantity of ammonia of 60 to 85% of the stoichiometric amount. The balance of the gaseous ammonia, also at a temperature near to that of the acid, is introduced laterally of the elongate vertical tubular chamber at any point, but preferably slightly below the restricted section of the cylindrical chamber.
Thus, the reactor can be conditioned to a nearly constant pressure at each and every point, and it has surprisingly been found that this prevents the formation of the incrustations or, at least, reduces them to virtually insignificant levels.
The shape of the reactor including the restricted section and the bottleneck portion, and the manner in which the ammonia is introduced, in addition to ensuring nearly the same pressure at every point, permits the reaction to be completed to the highest possible degree. The reaction heat can thus be exploited to the highest degree for attaining high levels of conversion of the acid of phosphorus to polyphosphoric acid. The temperature which can be attained in the reactor can reach 350 to 360"C, but it is preferred to carry out the reaction at a temperature slightly above 300"C.
In the accompanying drawing, there is shown, by way of example, an apparatus suitable for carrying out the process according to the present invention.
The apparatus shown in the drawing has a small cylindrical chamber 1, a bore 2 in which a spray nozzle for introducing the acid of phosphorus is inserted, a bore 3 through the wall of the small chamber 1 for introducing ammonia (e.g. 60 to 80% of the stoichiometric amount) when the ammonia is not introduced through the spray nozzle for introducing the acid of phosphorus, a restricted section 4, a bore 5 for introducing the remainder of the ammonia, an elongate vertical tubular chamber 6, and a port 7 through which the polyphosphate is discharged, the port 7 being immersed in a liquid contained in a collection tank 8. The drawing is an exploded view showing the manner in which the apparatus is constructed and assembled.
The polyphosphate exiting the apparatus shown in the drawing is promptly dissolved in the liquid contained in the collection tank 8, together with water vapour and unreacted ammonia.
The liquid in the collection tank is kept there for about 30 minutes, the time which is required for forming a homogenized mixture with the reactor effluent and for cooling. Longer times are not advisable since they would cause unnecessary losses of polyphosphates by hydrolysis thereof to orthophosphates.
The product of the apparatus shown in the drawing usually has a nitrogen content of 11 to 13% and a content of P205 of 58 to 64%, at least 50% of which is in the condensed form. The condensed form is normally present in an amount over 60% and can even attain as high levels as 80%.
The invention will now be illustrated by the following Examples.
EXAMPLE 1
A commercial grade phosphoric acid having a P205 content of 56.3% and a content of S04-- ions of 6.3% was fed into the reactor shown in the drawing at a rate of flow of 8.8 kg per hour and at a temperature of 1 35 C, and was reacted with gaseous ammonia fed in at a temperature of 1 35 C and at a rate of flow of 1.8 kg per hour. The first restriction of the reactor has a diameter of 2 mm and the final restricted section had a diameter of 1.5 mm, the pressure in the reactor being 1.5 kg/cm2 and the temperature being near to 300"C. About 85% of the ammonia, together with the acid, were fed into the reactor through bore 2, the balance of the ammonia being fed into the reactor through to the bore 5. The reactor melt was discharged and cooled to 45"C in the collection tank 8, to which filtered water was added at a rate of flow of 4.08 litres per hour. The final product had the following properties:
Total P205 34.1%
Ortho P205 13.2%
Ammoniacal nitrogen 10.2% pH (10% solution) 6.5
Specific gravity 1042 g/litre
Total polyphosphate (P205) 61.2%
Pyrophosphate (P205) 44%
Tripolyphosphate (P205) 13.7% Higher phosphates (P2Os) 3.5%.
EXAMPLE 2
By the same procedure as in Example 1, commercial grade phosphoric acid having a content of P205 of 60.1% and a content of S04-- ions of 6.2% has reacted, at a rate of flow of 8.95 kg per hour, with gaseous ammonia fed into the reactor at a rate of flow of 1.97 kg per hour. A pressure of 1.5 kg/cm2 was established in the reactor, and the temperature was 300"C. In the collecting tank, water was introduced at a rate of flow of 4.91 litres per hour.The end product had the following properties:
Total P2O5 34.0% Ortho P205 11.1% Ammoniacal nitrogen 10.3% pH (10% solution) 6.6
Specific gravity 1400 g/litre
Total polyphosphates 67.3%
Pyrophosphate (P205) 39.7% Tripolyphosphate (P205) 19.3% Higher poiyphosphates (P205) 8.3%.
EXAMPLE 3
A phosphoric acid having a content of P205 of to 60.1 % and a content of S04-- ions of 4%, to which no sulphuric acid had been added, was reacted with ammonia under the same conditions as in Example 2. The product obtained had the following properties:
Total P205 34.2%
Ortho P205 13.6%
Ammoniacal nitrogen 10.2% ph (10% solution) 6.5
Specific gravity 1401 g/litre
Total polyphosphates P205 60.2%
Pyrophosphate P205 43.7% Tripolyphosphate P205 10.3%
Higher polyphosphates P205 6.2%.
Example 4
A phosphoric acid having a P205 content of 61.7% and a content of S04-- ions of 4.9% was reacted, at a rate of flow of 8.95 kg per hour, with gaseous ammonia at a rate of flow of 2.03 kg per hour. About 80% of the ammonia was fed to the reactor through bore 2, whereas the balance of the ammonia was fed to the reactor through bore 5. In the reactor, the pressure was about 1.1 kg/cm2 while the temperature exceeded 300"C. In the collecting tank, water, maintained at a temperature of 47"C, was introduced at a rate of flow of 5.06 litres per hour.
The first and the second restricted sections of the reactor had the same size as in the previous
Examples. The product obtained had the following properties:
Total P2 O5 34.5%
Ortho P205 10.3%
Ammoniacal nitrogen 10.5% pH (10% solution) 6.5
Specific gravity at 20'C 1410 g/litre Total polyphosphates P205 70.8%
Pyrophosphate P205 36.4%
Tripolyphosphate P205 21.8%
Higher polyphosphates P205 12.6%.
Claims (17)
1. A process for the preparation of ammonium polyphosphate, which comprises reacting gaseous ammonia with an acid of phosphorus selected from orthophosphoric acid and/or superphosphoric acid in a vertical elongate reactor having a restricted section dividing the reactor into an upper restricted chamber and a lower elongate tubular chamber, the pressure in the reactor being from 1.3 to 6 atmospheres.
2. A process according to claim 1, wherein 60 to 80% of the total amount of ammonia is fed to the upper chamber and the balance of the ammonia is fed to the lower chamber.
3. A process according to claim 1 or 2, wherein the ammonia is fed to the upper chamber in admixture with the acid of phosphorus.
4. A process according to claim 1 or 2, wherein the ammonia is fed to the upper chamber separately from the acid of phosphorus.
5. A process according to any of claims 1 to 4, wherein the ammonia is fed to the lower chamber in the neighbourhood of the restricted section.
6. A process according to any of claims 1 to 5, wherein the acid of phosphorus has a P205 content of from 57% to 62% by weight.
7. A process according to any of claims 1 to 6, wherein the acid of phosphorus is one obtained by a wet treatment, and is used without purification.
8. A process according to any of claims 1 to 7, wherein the pressure in the reactor is substantially constant during the reaction.
9. A process according to any of claims 1 to 8, wherein the acid of phosphorus contains sulphuric acid in an amount of up to 15% by weight based on the weight of the acid of phosphorus.
1 0. A process according to any of claims 1 to 9, wherein the reaction product is discharged from the lower chamber and mixed with water.
11. A process according to any of claims 1 to 10, wherein the reactor is a reactor substantially as hereinbefore described with reference to, and as shown in, the accompanying drawing.
1 2. A process according to claim 1, substantially as described in any of the foregoing
Examples.
1 3. Ammonium polyphosphate prepared by a process according to any of claims 1 to 1 2.
1 4. An apparatus for use in carrying out a process according to claim 1, comprising a vertical elongate reactor having a restricted section dividing the reactor into an upper restricted chamber and a lower elongate tubular chamber, the lower chamber being terminated by another restricted section.
15. An apparatus as claimed in claim 14, wherein the upper chamber has, at or near the top thereof, a bore for the introduction of the acid of phosphorus, wherein the upper chamber has a further bore for the lateral introduction of gaseous ammonia, and wherein the lower chamber has a bore for the lateral introduction of gaseous ammonia.
16. An apparatus as claimed in claim 14 or 15, further comprising a vessel into which the lower portion of the reactor extends.
17. An apparatus as claimed in claim 14, substantially as hereinbefore described with reference to, and as shown in, the accompanying drawing.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT22562/80A IT1174670B (en) | 1980-06-05 | 1980-06-05 | PROCEDURE FOR THE PRODUCTION OF AMMONIUM POLYPHOSPHATES AND EQUIPMENT TO MAKE IT |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2077711A true GB2077711A (en) | 1981-12-23 |
| GB2077711B GB2077711B (en) | 1983-12-21 |
Family
ID=11197860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8116676A Expired GB2077711B (en) | 1980-06-05 | 1981-06-01 | Preparation of ammonium polyphosphate |
Country Status (5)
| Country | Link |
|---|---|
| BE (1) | BE889096A (en) |
| ES (1) | ES503253A0 (en) |
| GB (1) | GB2077711B (en) |
| IT (1) | IT1174670B (en) |
| MA (1) | MA19168A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2521544A1 (en) * | 1982-02-15 | 1983-08-19 | Vyzk Ustav Chem Tech | PROCESS FOR THE CONTINUOUS PREPARATION OF A FUSED MASS OF CONDENSED AMMONIUM PHOSPHATES AND DEVICE FOR CARRYING OUT SAID METHOD |
| EP0272974A2 (en) * | 1986-12-18 | 1988-06-29 | Grande Paroisse S.A. | Process of neutralisation of acids by ammoniac |
-
1980
- 1980-06-05 IT IT22562/80A patent/IT1174670B/en active
-
1981
- 1981-06-01 GB GB8116676A patent/GB2077711B/en not_active Expired
- 1981-06-02 ES ES503253A patent/ES503253A0/en active Granted
- 1981-06-02 MA MA19377A patent/MA19168A1/en unknown
- 1981-06-14 BE BE0/205000A patent/BE889096A/en not_active IP Right Cessation
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2521544A1 (en) * | 1982-02-15 | 1983-08-19 | Vyzk Ustav Chem Tech | PROCESS FOR THE CONTINUOUS PREPARATION OF A FUSED MASS OF CONDENSED AMMONIUM PHOSPHATES AND DEVICE FOR CARRYING OUT SAID METHOD |
| EP0272974A2 (en) * | 1986-12-18 | 1988-06-29 | Grande Paroisse S.A. | Process of neutralisation of acids by ammoniac |
| EP0272974A3 (en) * | 1986-12-18 | 1989-03-15 | Cdf Chimie Azote Et Fertilizants S.A. | Tubular reactor |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2077711B (en) | 1983-12-21 |
| IT1174670B (en) | 1987-07-01 |
| ES8203798A1 (en) | 1982-04-01 |
| ES503253A0 (en) | 1982-04-01 |
| IT8022562A0 (en) | 1980-06-05 |
| MA19168A1 (en) | 1981-12-31 |
| BE889096A (en) | 1981-12-04 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 19960601 |