CN100336846C - Production method of poly ammonium phosphate - Google Patents
Production method of poly ammonium phosphate Download PDFInfo
- Publication number
- CN100336846C CN100336846C CNB2004100796347A CN200410079634A CN100336846C CN 100336846 C CN100336846 C CN 100336846C CN B2004100796347 A CNB2004100796347 A CN B2004100796347A CN 200410079634 A CN200410079634 A CN 200410079634A CN 100336846 C CN100336846 C CN 100336846C
- Authority
- CN
- China
- Prior art keywords
- condensing agent
- polyphosphoric acid
- ammonium
- purity
- ammonium polyphosphate
- 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.)
- Expired - Fee Related
Links
Landscapes
- Fertilizers (AREA)
Abstract
The present invention discloses a method for producing poly ammonium phosphate. In the method, polyphosphoric acid is adopted as a raw material, a condensing agent is added to the polyphosphoric acid, and the weight ratio of the polyphosphoric acid to the condensing agent is 1: 1; after being uniformly mixed, the polyphosphoric acid and the condensing agent are added to a continuous type synthesis reactor, and reaction is continuously carried out for 5 to 210 minutes at the temperature from 100 DEG C to 500 DEG C under the pressure from 0.01MPa to 0.35MPa; and the high-purity ammonium polyphosphate of different polymerization degree is obtained. If the purity of the polyphosphoric acid is transformed to be different, then, a corresponding condensing agent is selected, and the required ammonium polyphosphate of different quality is obtained; and the condensing agent is selected from one type of urea, ammonium bicarbonate, melamine, dicyanodiamide and ammonium sulfate, or the mixture of the urea, the ammonium bicarbonate, the melamine, the dicyanodiamide and the ammonium sulfate.
Description
Technical field
The present invention relates to a kind of production method of ammonium polyphosphate, especially relate to a kind of production method of high purity high-polymerization degree ammonium polyphosphate.
Background technology
Ammonium polyphosphate is a kind of nitrogenous poly-phosphate.Different purposes according to product adopt different production methods and equipment thereof often.The water miscible product overwhelming majority of low polymerization degree is used as fertilizer and uses, and is used for fire retardant on a small quantity.High purity high-polymerization degree water-insoluble long-chain shape ammonium polyphosphate then is used to prepare senior frie retardant coating, flame retardant plastics.At present, the research in this field mainly is to carry out at acquisition high-polymerization degree high purity long chain shape, consistency ammonium polyphosphate product good, stay in grade.
In the prior art, normally used synthetic method is directly to mix with urea with ortho-phosphoric acid, control certain reaction temperature and reaction times, carries out condensation reaction and makes low polymerization degree (n ≈ 30), short chain shape product.This method products obtained therefrom is not high and As time goes on degraded can take place influenced its purposes owing to the polymerization degree.Simultaneously,, make that reaction process effusion exhausted air quantity is big owing to contain a large amount of free-waters in the ortho-phosphoric acid as raw material, huge to conversion unit material requirement height and treatment of waste gas system.And the sticking wall of reaction mass has influenced the mass-producing continuous production of this technology.Beginning to develop the ammonium polyphosphate product the domestic eighties, mainly adopt ortho-phosphoric acid---the urea condensation method is in small scale, situation that level is low always.Still there is not large-scale continuous industrial report.
In addition, as day the disclosure specially permit clear 49-30356: adopt ortho-phosphoric acid ammonium salt (as primary ammonium phosphate) and urea Hybrid Heating to dewater and produce the method for water-insoluble high purity high-polymerization degree ammonium polyphosphate product.Because its reaction process is slow, the production control difficulty, productive rate is low, and the energy consumption height is promoted thereby influenced its industrialized enforcement.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of high purity ammonium polyphosphate, this method has overcome the problems referred to above of ordinary method, and production control is convenient, the productive rate height, energy consumption is low, helps realizing large-scale continuous industrial production.
Purpose of the present invention is achieved by following technical proposals.
The invention provides a kind of production method of ammonium polyphosphate, this method adopts the step of following order:
(1) with polyphosphoric acid (H
N+2P
nO
3n+1) be raw material, add condensing agent then, the weight ratio of polyphosphoric acid and condensing agent is 1: 1, and both are mixed;
(2) gains of step (1) are added in the continuous synthetic reactor, at 100 ℃～500 ℃, with under the pressure of 0.01MPa～0.35MPa, sustained reaction 5～210 minutes promptly obtains the high purity ammonium polyphosphate of different polymerization degree;
(3) with the different purity of polyphosphoric acid conversion in the step (1), select corresponding condensing agent, can obtain the ammonium polyphosphate of required different qualities.
Described raw material polyphosphoric acid (H
N+2P
nO
3n+1) purity (with H
3PO
4Meter) weight percentage is 90%～120%;
Described condensing agent is selected from a kind of in urea, bicarbonate of ammonia, trimeric cyanamide, Dyhard RU 100, the ammonium sulfate or their mixture.
The present invention compared with prior art has following beneficial effect:
(1) be raw material with polyphosphoric acid and condensing agent, adopt the continuous process technology, reduced processing step, improved the requirement of process stream equipment material, little to influence degree.Can obtain the ammonium polyphosphate product of high purity high-polymerization degree easily.The employing polyphosphoric acid is a raw material, and the impurity level of bringing system into is few, and simultaneously, polyphosphoric acid does not contain free-water, has not only guaranteed the carrying out of building-up reactions but also reduced energy consumption, has also alleviated the corrosion of material to equipment material simultaneously.
(2) reduce the tail gas amount of synthetic reaction process, reduced the investment of tail gas treatment device.Because adopt the raw material difference, the present invention's discharge tail gas amount in synthetic reaction process has reduced 50%; Tail gas is reclaimed makes other phosphate product or byproduct.Have favorable economic benefit and social benefit.
(3) adopt continuous process, guaranteed the stable of quality product, reduced productive labor intensity, improved working condition.And prior art often adopts batch process, and industrial scale is little, and labour intensity is big, and because technological operation personnel's technological disparity, it is stable to cause quality product to be difficult for.
(4) can be by changing the ammonium polyphosphate product of process control condition production different purity different polymerization degree in same set of device.
Embodiment
By specific embodiments of the invention given below, can further be well understood to the present invention.But they are not limitation of the invention.
Except as otherwise noted, the percentage ratio that is adopted among the present invention is weight percentage.
Embodiment 1
Polyphosphoric acid with 1 weight part is a raw material, polyphosphoric acid (H
N+2P
nO
3n+1) purity is (with H
3PO
4Meter) weight percentage is 100%; Add 1 weight part urea as condensing agent, join in the continuous synthetic reactor after the two is mixed, at 500 ℃, 0.35MPa condition under, reaction can obtain 1 weight part, white crystal shape high purity (99.5%), high-polymerization degree (n 〉=250) ammonium polyphosphate product more than 210 minutes.
Embodiment 2～embodiment 5
Except described condensing agent was selected from a kind of in bicarbonate of ammonia, trimeric cyanamide, Dyhard RU 100, the ammonium sulfate respectively, other process was with embodiment 1.
Embodiment 6
Except the mixture of described condensing agent employing urea and bicarbonate of ammonia, urea 70%, bicarbonate of ammonia are outside 30%, and other process is with embodiment 1.
Embodiment 7
Except the mixture of described condensing agent employing trimeric cyanamide and ammonium sulfate, trimeric cyanamide 90%, ammonium sulfate are outside 10%, and other process is with embodiment 1.
Embodiment 8
Except the mixture of described condensing agent employing trimeric cyanamide and urea, trimeric cyanamide 30%, urea are outside 70%, and other process is with embodiment 1.
Embodiment 9
Except the mixture of described condensing agent employing Dyhard RU 100, trimeric cyanamide and ammonium sulfate, Dyhard RU 100 70% trimeric cyanamide 25%, ammonium sulfate is outside 5%, other process is with embodiment 1.
Embodiment 10
Except the mixture of described condensing agent employing urea and ammonium sulfate, urea 90%, ammonium sulfate are outside 10%, and other process is with embodiment 1
Embodiment 11
Except the mixture of described condensing agent employing bicarbonate of ammonia, trimeric cyanamide and urea, trimeric cyanamide 70%, urea 25%, bicarbonate of ammonia are outside 5%, other process is with embodiment 1.
Embodiment 12
Repeat embodiment 1, the change condition is 100 ℃ of temperature, pressure 0.01MPa, and the reaction times can obtain 1.15 weight parts more than 5 minutes, and white crystal shape purity is 90%, and the polymerization degree is the ammonium polyphosphate product of n≤20.
Embodiment 13
Repeat embodiment 12, change polyphosphoric acid (H
N+2P
nO
3n+1) purity is (with H
3PO
4Meter) weight percentage is 90%, and the reaction times can obtain 1.02 weight parts more than 90 minutes, and white crystal shape purity is 90%, and the polymerization degree is the ammonium polyphosphate product of n≤20.
Embodiment 14
Repeat embodiment 1, change polyphosphoric acid (H
N+2P
nO
3n+1) purity is (with H
3PO
4Meter) weight percentage is 105%, and working condition is 200 ℃ of temperature, pressure 0.15MPa, and the reaction times can obtain 1.11 weight parts more than 60 minutes, and white crystal shape purity is 95%, and the polymerization degree is the ammonium polyphosphate product of n 50.
Embodiment 15
Repeat embodiment 1, the change condition is 300 ℃ of temperature, pressure 0.25MPa, and the reaction times can obtain 1.03 weight parts more than 120 minutes, and white crystal shape purity 97%, the polymerization degree are the ammonium polyphosphate product of n≤80.
Embodiment 16
Repeat embodiment 1, change polyphosphoric acid (H
N+2P
nO
3n+1) purity is (with H
3PO
4Meter) weight percentage is 90%, and processing condition are 300 ℃ of temperature, pressure 0.30MPa, and the reaction times can obtain 0.95 weight part more than 180 minutes, and white crystal shape purity is 95%, and the polymerization degree is the ammonium polyphosphate product of n≤50n.
Embodiment 17
Repeat embodiment 1, the change condition is 400 ℃ of temperature, pressure O.30MPa, the reaction times can obtain 1.01 weight parts more than 180 minutes, white crystal shape purity is 98.5%, the polymerization degree is the ammonium polyphosphate product of n 〉=120.
Embodiment 18
Repeat embodiment 1, change polyphosphoric acid (H
N+2P
nO
3n+1) purity is (with H
3PO
4Meter) weight percentage is 115%, and processing condition are 400 ℃ of temperature, pressure 0.30MPa, and the reaction times can obtain 1.16 weight parts more than 60 minutes, and white crystal shape purity is 98.5%, and the polymerization degree is the ammonium polyphosphate product of n 120.
Claims (1)
1. the production method of an ammonium polyphosphate, this method adopts the step of following order:
(1) be raw material with the polyphosphoric acid, add condensing agent then, the weight ratio of polyphosphoric acid and condensing agent is 1: 1, and both are mixed; By ortho-phosphoric acid, the weight percentage of described raw material polyphosphoric acid purity is 90%～115%; Described condensing agent is selected from a kind of in urea, bicarbonate of ammonia, melamine, Dyhard RU 100 or the ammonium sulfate or their mixture;
(2) gains of step (1) are added in the continuous synthetic reactor, under 100 ℃～500 ℃ and 0.01MPa～0.35MPa condition, sustained reaction 5～210 minutes promptly obtains the ammonium polyphosphate of different polymerization degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100796347A CN100336846C (en) | 2004-12-23 | 2004-12-23 | Production method of poly ammonium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100796347A CN100336846C (en) | 2004-12-23 | 2004-12-23 | Production method of poly ammonium phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1651488A CN1651488A (en) | 2005-08-10 |
| CN100336846C true CN100336846C (en) | 2007-09-12 |
Family
ID=34869120
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100796347A Expired - Fee Related CN100336846C (en) | 2004-12-23 | 2004-12-23 | Production method of poly ammonium phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100336846C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101700879B (en) * | 2009-11-20 | 2011-03-23 | 华东理工大学 | Method for preparing crystalline V-type ammonium polyphosphate with phosphoric acid |
| CN101830449A (en) * | 2010-05-11 | 2010-09-15 | 云南省化工研究院 | Method for producing ammonium polyphosphate by using stepwise reaction and polymerization |
| CN103373717B (en) * | 2012-04-23 | 2016-04-20 | 防城港博森化工科技股份有限公司 | A kind of preparation method of the low-polymerization-dammonium ammonium polyphosphate aqueous solution |
| CN102976300B (en) * | 2012-08-23 | 2014-04-16 | 云南天耀化工有限公司 | Method for preparing crystal II type ammonium polyphosphate by using polyphosphoric acid |
| CN105859330A (en) * | 2015-04-02 | 2016-08-17 | 贵州芭田生态工程有限公司 | A polyphosphate and a low-temperature preparing method thereof |
| CN105776167A (en) * | 2015-04-02 | 2016-07-20 | 贵州芭田生态工程有限公司 | Polyphosphate and preparation method thereof |
| CN105293464B (en) * | 2015-11-25 | 2017-07-21 | 西南科技大学 | A kind of method of the synthetic-highly polymerized degree APP of HTHP |
| CN106220249A (en) * | 2016-07-12 | 2016-12-14 | 贵州芭田生态工程有限公司 | The preparation method of Quadrafos compound fertilizer |
| CN114773129B (en) * | 2022-04-25 | 2023-08-11 | 什邡市长丰化工有限公司 | Hard water resistant water-soluble fertilizer and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030625A (en) * | 1987-07-16 | 1989-01-25 | 北京市朝阳区来广营有机化工厂 | Fire retardant agent for products of natural fibres and processing method thereof |
| CN1030779A (en) * | 1987-07-17 | 1989-02-01 | 北京建筑防火材料喷涂工程公司 | Expansible fireproof decorative coating for steel structure |
| CN1112339C (en) * | 1999-12-23 | 2003-06-25 | 胡光霞 | Foliage fertilizer |
-
2004
- 2004-12-23 CN CNB2004100796347A patent/CN100336846C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1030625A (en) * | 1987-07-16 | 1989-01-25 | 北京市朝阳区来广营有机化工厂 | Fire retardant agent for products of natural fibres and processing method thereof |
| CN1030779A (en) * | 1987-07-17 | 1989-02-01 | 北京建筑防火材料喷涂工程公司 | Expansible fireproof decorative coating for steel structure |
| CN1112339C (en) * | 1999-12-23 | 2003-06-25 | 胡光霞 | Foliage fertilizer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1651488A (en) | 2005-08-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1317190C (en) | High-Al13 aluminium trichloride polymer crystal and its prepn | |
| CN100336846C (en) | Production method of poly ammonium phosphate | |
| CN103382092B (en) | A kind of preparation method of naphthalene water reducer | |
| CN1793065A (en) | Process for producing slow releasing silicon potassium compound fertilizer by potassium feldspar | |
| CN104790024A (en) | Preparation method for aragonite calcium carbonate whisker with high length-diameter ratio | |
| CN108408751A (en) | A method of preparing purity calcium carbonate using ardealite ammonia process trapping carbon dioxide | |
| CN101830449A (en) | Method for producing ammonium polyphosphate by using stepwise reaction and polymerization | |
| CN101066771A (en) | Microwave radiation process for producing potassium sulfate | |
| CN1872669A (en) | Method for producing diammonium phosphate by concentrating acid slime, and secondary ammoniation reactor | |
| CN101486481A (en) | Method for coproduction of ammonia sulfate and superfine light calcium carbonate from fluorgypsum | |
| CN1872799A (en) | Associated production method by using condensed phosphoric acid to produce diammonium phosphate, and by using condensed acidic feed pulp to produce phosphor ammonium or/and compound fertilizer | |
| CN108796612B (en) | Method for preparing calcium sulfate whisker and co-producing ammonium sulfate by phosphogypsum cyclic decomposition | |
| CN101041603A (en) | Preparation technical method of urine sulfur radical composite fertilizer | |
| CN112321456B (en) | Evaporation method of caprolactam in process for preparing 6-aminocapronitrile from caprolactam in gas phase | |
| CN103224416A (en) | Synthetic method of ammonium zinc phosphate slow release fertilizer | |
| CN108439451A (en) | The method for preparing precipitated calcium carbonate using ardealite | |
| CN1238308C (en) | Method for preparing chemical fertilizer from salt-making mother liquor (bittern) or salt water | |
| CN115849959B (en) | Organic acid modified urea formaldehyde slow-release nitrogenous fertilizer and reactive extrusion low-cost preparation process thereof | |
| CN1043521C (en) | Method and apparatus for tower wet production process of concentrated phosphoric acid | |
| WO2006111057A1 (en) | A method for comprehensively using of the raw material in wet-processing phosphorite and producing nano calcium carbonate with high purity and microsphere shape at the same time | |
| CN1044458C (en) | Method for producing calcium hydrophosphate and monocalcium phosphate as feeds | |
| CN106350870A (en) | Disposal and utilization method for sulfuric acid waste liquid | |
| CN1363511A (en) | Process for preparing fluorine compound and SiO2 from sodium fluosilicate | |
| CN1082001A (en) | The preparation vitriolate of tartar in and synthesis method | |
| CN115925644B (en) | Method for preparing flame retardant by using amine waste mother liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070912 Termination date: 20201223 |