CN102674287A - Method for producing ammonium polyphosphate flame retardant by utilizing melamine tail gas - Google Patents
Method for producing ammonium polyphosphate flame retardant by utilizing melamine tail gas Download PDFInfo
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- CN102674287A CN102674287A CN2012101281431A CN201210128143A CN102674287A CN 102674287 A CN102674287 A CN 102674287A CN 2012101281431 A CN2012101281431 A CN 2012101281431A CN 201210128143 A CN201210128143 A CN 201210128143A CN 102674287 A CN102674287 A CN 102674287A
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- tail gas
- ammonium polyphosphate
- flame retardant
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- melamine
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Abstract
The invention relates to a method for producing an ammonium polyphosphate flame retardant by utilizing melamine tail gas, which comprises the following steps: utilizing ammonia gas in the melamine tail gas as a raw material, introducing the tail gas containing the ammonia gas into a reactor, reacting with heated phosphoric acid or polyphosphoric acid, raising the temperature to 240-350 DEG C, maintaining for 15-120 minutes till viscous liquid is formed, stopping introducing the melamine tail gas, and cooling, washing and drying at a high speed to obtain the ammonium polyphosphate with a polymerization degree of 30-400. After reaction, the tail gas in the reactor is continuously introduced into an ammonium bicarbonate production device to obtain ammonium bicarbonate. The melamine tail gas can be produced by a high-pressure, medium-pressure and low-pressure melamine device. The method has the beneficial effects that the melamine tail gas is changed by melamine production enterprises from wastes into valuables, and a more economic and more environmentally-friendly ammonium polyphosphate flame retardant production method is provided for ammonium polyphosphate flame retardant enterprises.
Description
Technical field
The present invention relates to a kind of working method of ammonium polyphosphate, relate in particular to a kind of method of utilizing melamine tail gas to produce ammonium polyphosphate flame retardant.
Background technology
Ammonium polyphosphate is a kind of environmentally friendly efficient flame-retarding agent of generally acknowledging both at home and abroad.Because it is not halogen-containing, do not contain heavy metal element, when burning, smokeless, nontoxic, no molten drop, and be widely used in frie retardant coating, plastics, fiber, resin, timber, etc. various fields.Especially after after finding the burning of halogen product the eighties in last century, can giving off poisonous gas, traditional halogen flame retardant products is replaced by polyphosphoric acid type flame retardant in many occasions.
Trimeric cyanamide is the important industrial chemicals of synthetic paint, resin, paint.Along with domestic and international raising to environmental requirement.Trimeric cyanamide is as the important source material of environmentally friendly machine, and the demand of trimeric cyanamide increases sharply.The industrial scale of trimeric cyanamide enterprise also enlarges rapidly.For Melamine Production enterprise, how to handle a large amount of melamine tail gas that produce in the Melamine Production process, not only be related to Production of Cyanuramide cost problem, also be related to the protection problem of environment.The processing of melamine tail gas be each trimeric cyanamide enterprise the key subjects that must face.The present invention is exactly the treatment process that a kind of brand-new melamine tail gas will be provided for trimeric cyanamide enterprise.
The Production of Cyanuramide principle is at high temperature to drop into urea, and urea decomposes under high-temperature condition emits ammonia and CO
2, under the effect of catalyzer, the acceleration molecular reorganization forms trimeric cyanamide, ammonia and CO more than needed simultaneously
2Discharge as tail gas.According to this principle, main composition is NH in the melamine tail gas
3And CO
2Our method is to produce ammonium polyphosphate flame retardant through the ammonia that phosphoric acid absorbs in the melamine tail gas, again with the CO that contains of remainder
2Tail gas send into carbon ammonium device and produce the carbon ammonium, realize zero release.This method has not only reduced the Production of Cyanuramide cost, also increases the melamine tail gas value-added content of product, has also reduced the production cost of ammonium polyphosphate flame retardant, has also avoided the pollution of melamine tail gas to environment.
Summary of the invention
Technical problem:The invention provides a kind of method of utilizing melamine tail gas to produce ammonium polyphosphate flame retardant, efficiently utilize the NH in the tail gas
3, the production cost of reduction trimeric cyanamide, ammonium polyphosphate flame retardant; Simultaneously with the CO that contains after the polyreaction
2Tail gas continue to be passed into carbon ammonium production equipment, utilize the CO in the melamine tail gas
2Produce the carbon ammonium, reduce the production cost of carbon ammonium; The present invention fully absorbs NH in the melamine tail gas
3And CO
2, reduce the pollution of melamine tail gas to environment, realize zero release.
Technical scheme:A kind of method of utilizing melamine tail gas to produce ammonium polyphosphate flame retardant comprises the steps:
(1), phosphoric acid, polyphosphoric acid or both mixtures dropped into reaction kettle after, heat up, temperature is controlled in the 80-120 ℃ of scope;
(2), melamine tail gas is passed in the reaction kettle, with phosphoric acid or polyphosphoric acid reaction, temperature of reaction is in 240-350 ℃ of scope, and the reaction times is 15-120min;
(3), cooling, washing, drying obtain ammonium polyphosphate, the polymerization degree is between 30-400.
Phosphoric acid described in the step (1) is phosphoric acid by wet process or dry method phosphoric acid.
The polymerization degree of polyphosphoric acid is no more than 4 described in the step (1).
The mixing of phosphoric acid and polyphosphoric acid can mix for arbitrary proportion in the step (1).
Intensification temperature described in the step (1) is controlled in the 85-95 ℃ of scope.
Melamine tail gas described in the step (2) be high-pressure process or middle-pressure process or low-pressure process produce that trimeric cyanamide produced contain ammonia and CO
2Tail gas, TR is between 10~300 ℃.
Temperature of reaction described in the step (2) is in 290-300 ℃ of scope, and the reaction times is 30-60min.Reaction continues to be passed into carbon ammonium production equipment with tail gas in the reaction kettle after finishing, and obtains the carbon ammonium.
Described ammonium polyphosphate, the polymerization degree are between 30-400, and wherein the low polymerization degree ammonium polyphosphate can be used as the long-acting fertilizer use, and the high-polymerization degree ammonium polyphosphate can be used as fire retardants such as coating, plastics, resin, timber and uses.
Beneficial effect:The present invention utilizes melamine tail gas to produce the method for ammonium polyphosphate flame retardant, efficiently utilizes the NH in the tail gas
3, the production cost of reduction ammonium polyphosphate flame retardant; Reduce the pollution of melamine tail gas simultaneously to environment.Simultaneously the tail gas that contains CO2 after the polyreaction is continued to be passed into carbon ammonium production equipment, utilize the CO in the melamine tail gas
2Produce the carbon ammonium, reduce the production cost of carbon ammonium; The present invention fully absorbs NH in the melamine tail gas
3And CO
2, reduce the pollution of melamine tail gas to environment, realize zero release.
Description of drawings
Fig. 1 produces the ammonium polyphosphate schema for melamine tail gas.
Embodiment
Below in conjunction with accompanying drawing the present invention is further specified.
Embodiment 1
With the polymerization degree is that 4 polyphosphoric acid drops in the reaction kettle, be warming up to 80 ℃ after, what feed that high-pressure process produces that trimeric cyanamide produced contains ammonia and CO
2Tail gas, NH
3Absorbed by polyphosphoric acid, temperature of reaction is at 350 ℃, and the reaction times is 15min; Cooling, washing obtains ammonium polyphosphate, and the polymerization degree is between 30-400.
The CO of remainder in the tail gas
2Output to carbon ammonium device and produce the carbon ammonium, realize the NH in the melamine tail gas
3And CO
2Make full use of, obtain ammonium polyphosphate flame retardant, carbon ammonium product, realize zero release environment.
Embodiment 2
Phosphoric acid by wet process is dropped in the reaction kettle, be warming up to 120 ℃ after, what feed middle-pressure process production trimeric cyanamide produced contains ammonia and CO
2Tail gas, NH
3Absorbed by phosphoric acid, temperature of reaction is at 290 ℃, and the reaction times is 60min; Cooling, washing obtains ammonium polyphosphate, and the polymerization degree is between 30-400.
The CO of remainder in the tail gas
2Output to carbon ammonium device and produce the carbon ammonium, realize the NH in the melamine tail gas
3And CO
2Make full use of, obtain ammonium polyphosphate flame retardant, carbon ammonium product, realize zero release environment.
Embodiment 3
With dry method phosphoric acid and the polymerization degree is that 2 polyphosphoric acid mixture is that 3:1 drops in the reaction kettle with the mass ratio, be warming up to 85 ℃ after, what feed that low-pressure process produces that trimeric cyanamide produced contains ammonia and CO
2Tail gas, NH
3Absorbed by phosphoric acid and polyphosphoric acid mixture, temperature of reaction is at 300 ℃, and the reaction times is 30min; Cooling, washing obtains ammonium polyphosphate, and the polymerization degree is between 30-400.
The CO of remainder in the tail gas
2Output to carbon ammonium device and produce the carbon ammonium, realize the NH in the melamine tail gas
3And CO
2Make full use of, obtain ammonium polyphosphate flame retardant, carbon ammonium product, realize zero release environment.
Embodiment 4
With phosphoric acid by wet process and the polymerization degree is that 3 polyphosphoric acid mixture is that 1:3 drops in the reaction kettle with the mass ratio, be warming up to 95 ℃ after, what feed that low-pressure process produces that trimeric cyanamide produced contains ammonia and CO
2Tail gas, NH
3Absorbed by phosphoric acid and polyphosphoric acid mixture, temperature of reaction is at 240 ℃, and the reaction times is 120min; Cooling, washing obtains ammonium polyphosphate, and the polymerization degree is between 30-400.
The CO of remainder in the tail gas
2Output to carbon ammonium device and produce the carbon ammonium, realize the NH in the melamine tail gas
3And CO
2Make full use of, obtain ammonium polyphosphate flame retardant, carbon ammonium product, realize zero release environment.
The above only is a preferred implementation of the present invention; Be noted that for those skilled in the art; Under the prerequisite that does not break away from the principle of the invention, can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (7)
1. a method of utilizing melamine tail gas to produce ammonium polyphosphate flame retardant is characterized in that comprising the steps:
(1), phosphoric acid, polyphosphoric acid or both mixtures dropped into reaction kettle after, heat up, temperature is controlled in the 80-120 ℃ of scope;
(2), melamine tail gas is passed in the reaction kettle, with phosphoric acid or polyphosphoric acid reaction, temperature of reaction is in 240-350 ℃ of scope, and the reaction times is 15-120min;
(3), cooling, washing, drying obtain ammonium polyphosphate, the polymerization degree is between 30-400.
2. the method for utilizing melamine tail gas to produce ammonium polyphosphate flame retardant according to claim 1, it is characterized in that: the phosphoric acid described in the step (1) is phosphoric acid by wet process or dry method phosphoric acid.
3. the method for utilizing melamine tail gas to produce ammonium polyphosphate flame retardant according to claim 1, it is characterized in that: the polymerization degree of polyphosphoric acid is no more than 4 described in the step (1).
4. the method for utilizing melamine tail gas to produce ammonium polyphosphate flame retardant according to claim 1, it is characterized in that: the intensification temperature described in the step (1) is controlled in the 85-95 ℃ of scope.
5. the method for utilizing melamine tail gas to produce ammonium polyphosphate flame retardant according to claim 2 is characterized in that: the melamine tail gas described in the step (2) be high-pressure process or middle-pressure process or low-pressure process produce that trimeric cyanamide produced contain ammonia and CO
2Tail gas, TR is between 10~300 ℃.
6. the method for utilizing melamine tail gas to produce ammonium polyphosphate flame retardant according to claim 2, it is characterized in that: the temperature of reaction described in the step (2) is in 290-300 ℃ of scope, and the reaction times is 30-60min.
7. the method for utilizing melamine tail gas to produce ammonium polyphosphate flame retardant according to claim 1 is characterized in that: after step (2) reaction finishes tail gas in the reaction kettle is continued to be passed into carbon ammonium production equipment, obtain the carbon ammonium.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104528682A (en) * | 2014-12-18 | 2015-04-22 | 防城港博森化工有限公司 | Method for preparing full water-soluble ammonium polyphosphate water solution by using wet process phosphoric acid |
CN105084337A (en) * | 2015-09-07 | 2015-11-25 | 云南省化工研究院 | Polyphosphoric acid catalytic method for synthetizing crystalized II-type APP (ammonium polyphosphate) |
CN105347323A (en) * | 2015-12-15 | 2016-02-24 | 防城港博森化工科技股份有限公司 | Method of preparing ammonium polyphosphate by using phosphoric acid by wet process and yellow phosphorus as raw materials |
CN109054081A (en) * | 2018-06-14 | 2018-12-21 | 云南江磷集团股份有限公司 | Novel nitrogen phosphorus synergistic flame retardant and preparation method thereof |
CN113582201A (en) * | 2021-08-20 | 2021-11-02 | 四川金象赛瑞化工股份有限公司 | Process for recycling tail gas of cyanamide process |
Citations (4)
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US3382059A (en) * | 1964-07-02 | 1968-05-07 | Tennessee Valley Authority | Production of ammonium polyphosphates from wet process phosphoric acid |
US3695835A (en) * | 1970-05-06 | 1972-10-03 | Tommy Carter Kearns | Ammonium polyphosphate manufacture |
CN101029235A (en) * | 2006-02-27 | 2007-09-05 | 江苏绿陵化工集团 | Production of electron triammonium polyphosphate fire retardant |
CN102139865A (en) * | 2011-03-22 | 2011-08-03 | 华东理工大学 | Preparation method for crystallization type II ammonium polyphosphate by non-condensing agent technology |
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2012
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US3382059A (en) * | 1964-07-02 | 1968-05-07 | Tennessee Valley Authority | Production of ammonium polyphosphates from wet process phosphoric acid |
US3695835A (en) * | 1970-05-06 | 1972-10-03 | Tommy Carter Kearns | Ammonium polyphosphate manufacture |
CN101029235A (en) * | 2006-02-27 | 2007-09-05 | 江苏绿陵化工集团 | Production of electron triammonium polyphosphate fire retardant |
CN102139865A (en) * | 2011-03-22 | 2011-08-03 | 华东理工大学 | Preparation method for crystallization type II ammonium polyphosphate by non-condensing agent technology |
Non-Patent Citations (1)
Title |
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张健: "聚磷酸铵合成工艺研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》, no. 08, 31 December 2005 (2005-12-31) * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104528682A (en) * | 2014-12-18 | 2015-04-22 | 防城港博森化工有限公司 | Method for preparing full water-soluble ammonium polyphosphate water solution by using wet process phosphoric acid |
CN105084337A (en) * | 2015-09-07 | 2015-11-25 | 云南省化工研究院 | Polyphosphoric acid catalytic method for synthetizing crystalized II-type APP (ammonium polyphosphate) |
CN105347323A (en) * | 2015-12-15 | 2016-02-24 | 防城港博森化工科技股份有限公司 | Method of preparing ammonium polyphosphate by using phosphoric acid by wet process and yellow phosphorus as raw materials |
CN109054081A (en) * | 2018-06-14 | 2018-12-21 | 云南江磷集团股份有限公司 | Novel nitrogen phosphorus synergistic flame retardant and preparation method thereof |
CN113582201A (en) * | 2021-08-20 | 2021-11-02 | 四川金象赛瑞化工股份有限公司 | Process for recycling tail gas of cyanamide process |
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Application publication date: 20120919 |