CN108059141A - A kind of preparation method of II type ammonium polyphosphate fire proofing - Google Patents
A kind of preparation method of II type ammonium polyphosphate fire proofing Download PDFInfo
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- CN108059141A CN108059141A CN201711199157.1A CN201711199157A CN108059141A CN 108059141 A CN108059141 A CN 108059141A CN 201711199157 A CN201711199157 A CN 201711199157A CN 108059141 A CN108059141 A CN 108059141A
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- ammonium polyphosphate
- preparation
- fire proofing
- type ammonium
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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
- C09K21/04—Inorganic materials containing phosphorus
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention provides a kind of preparation methods of II type ammonium polyphosphate fire proofing：By weight, 100 parts of diammonium hydrogen phosphates and 80 110 parts of phosphorus pentoxides, 5 20 parts of urea, 14 parts of dodecanamide propyl sulfobetaines, 5 20 portions of ammonia buffer solutions carry out synthetic reaction, and product is using filter, washing, drying crushes, had both obtained II type ammonium polyphosphate fire proofing.
Description
Technical field
The present invention relates to a kind of preparation method of ammonium polyphosphate, especially a kind of preparation of II type ammonium polyphosphate fire proofing
Method.
Background technology
The performances such as heat-resisting quantity, water resistance, the weatherability of crystal II-type ammonium polyphosphate are the most excellent, therefore crystallization II-type gathers
Ammonium phosphate is in medium and high classes expanding fire-proof paint, plastics, unsaturated-resin, fabric, leather, rubber, paper, timber, fiber etc.
Flame retardant area have a wide range of applications, particularly its have it is nontoxic, do not drip, low smog the characteristics of, be currently on the market
The favorable substitutes of the most commonly used halogen flame of dosage.
CN106629647A disclose be related to it is a kind of prepare the new method of crystal II-type ammonium polyphosphate using thiocarbamide as condensing agent,
Include following steps：Ammonium dihydrogen phosphate and thiocarbamide are uniformly mixed, heating makes raw material by melting, foaming, solidification process；Powder
It is broken, it is continuously heating to and stirs, the sulfide gas of reaction generation is constantly replaced with dry air；Continue to heat, be passed through wet ammonia,
And be constantly stirred, ammonification makes its transformation of crystal, obtains product, is cooled to room under identical wet ammonia atmosphere protection afterwards
Temperature smashes, grinding obtains crystal II-type ammonium polyphosphate.
CN102139865A is related to a kind of preparation method of crystal form II ammonium polyphosphate, only with phosphoric acid, ammonium dihydrogen phosphate or
Any one or above-mentioned several mixtures in diammonium hydrogen phosphate are raw material, without additional condensing agent, by controlling reaction condition, are made
Standby crystal form II ammonium polyphosphate, prepared product stable crystal form, broken, yield is high.Advantages of the present invention：Without using five oxygen
Change two phosphorus as raw material, avoid the production high energy consumption of phosphorus pentoxide process route, the shortcomings of operating process is dangerous；Without using outer
Add condensing agent, without foamed phenomenon in preparation process, improve the utilization rate and production efficiency of equipment.
The a. that CN102976300B is achieved through the following technical solutions is using polyphosphoric acid, ammonium phosphate salt, urea as anti-
Raw material is answered to be added in after measuring in the reactor with stirring slurry and chuck temperature control, stirring temperature control is completely melt material, then adds again
Enter reaction promoter and compound modifying agent after metering, be completely melt, continue insulated and stirred and cure 30 minutes；B. by step a
Material be transferred in another reactor with roller-crushing mill pinch roller and chuck heat-conducting oil heating after completion of the reaction, pressurize cooling after
It is grinding to obtain crystal II-type ammonium polyphosphate.The present invention is by polyphosphoric acid raw material, using polyphosphoric acid and ammonium phosphate salt and urea
Reaction, and adds reaction promoter and compound modifying agent, and through polymerizeing and turning crystallization stable quality is obtained after melt-blended
Crystal II-type ammonium polyphosphate product enriches the Material synthesis route of crystal II-type ammonium polyphosphate product.
Currently, all it is to be using phosphorus pentoxide and diammonium hydrogen phosphate in high polymerization degree APP production both domestic and external
Basic material synthesis, but because the reaction is extremely violent, temperature rising is extremely rapid, causes the control of building-up process temperature
Very difficult, this reason so that the product degree of polymerization of synthesis is integrally relatively low.
The content of the invention
Present invention aims at the above-mentioned technical problems in the prior art are solved, a kind of II type ammonium polyphosphate resistance is provided
The preparation method of combustible material.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that：A kind of II type ammonium polyphosphate fire proofing
Preparation method, it is characterised in that preparation process includes：
（1）The preparation of ammonia buffer solution
By weight, 0.1-0.5 portions of lithium nitrate buffer solutions, 0.01-0.1 parts of 6- bromomethyl -3,4- dihydro -2- methyl-quinazolines -
4- ketone, 100 parts of liquefied ammonia mix 1-5h.
（2）Synthetic reaction
By weight, 100 parts of diammonium hydrogen phosphates and 80-110 parts of phosphorus pentoxides, 5-20 parts of urea, 1-4 parts of dodecanamide propyls
Sulfobetaines, 5-20 portions of ammonia buffer solutions carry out synthetic reaction, and product dries using filter, washing, crushes, both obtained II type
Ammonium polyphosphate fire proofing.
250~320 DEG C of the synthesis reaction temperature.
The synthesising reacting time 1-5h.
The lithium nitrate buffer solution, 6- bromomethyl -3,4- dihydro -2- methyl-quinazoline -4- ketone are commercial product.
The diammonium hydrogen phosphate, phosphorus pentoxide, urea, dodecanamide propyl sulfobetaines are commercial product.
The present invention is by adopting the above-described technical solution, have the advantages that：
By adding in ammonia buffer solution, avoid and be passed through ammonia and adversely affected caused by process unit, ammonia buffer solution gathers melting
The reaction heat of conjunction reduces, and makes the polymerisation of II type ammonium polyphosphate evenly, reacting balance, building-up process easy control of temperature,
The product degree of polymerization of synthesis is improved.
Specific embodiment
Following instance is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
Embodiment 1：
（1）The preparation of ammonia buffer solution
By weight, 0.2 portion of lithium nitrate buffer solution, 0.03 part of 6- bromomethyl -3,4- dihydro -2- methyl-quinazoline -4- ketone,
100 parts of liquefied ammonia mix 3h.
（2）Synthetic reaction
By weight, 100 parts of diammonium hydrogen phosphates and 90 parts of phosphorus pentoxides, 15 parts of urea, 2 parts of dodecanamide propyl sulfobetaines
Alkali, 11 portions of ammonia buffer solutions carry out synthetic reaction, and product is dried, crushed, both obtained the resistance of II type ammonium polyphosphate using filter, washing
Combustible material.Product identification M-1.
Embodiment 2：
（1）The preparation of ammonia buffer solution
By weight, 0.1 portion of lithium nitrate buffer solution, 0.01 part of 6- bromomethyl -3,4- dihydro -2- methyl-quinazoline -4- ketone,
100 parts of liquefied ammonia mix 1h.
（2）Synthetic reaction
By weight, 100 parts of diammonium hydrogen phosphates and 80 parts of phosphorus pentoxides, 5 parts of urea, 1 part of dodecanamide propyl sulfobetaines
Alkali, 5 portions of ammonia buffer solutions carry out synthetic reaction, and product is dried, crushed, both obtained the resistance of II type ammonium polyphosphate using filter, washing
Combustible material.Product identification M-2.
Embodiment 3：
（1）The preparation of ammonia buffer solution
By weight, 0.5 portion of lithium nitrate buffer solution, 0.1 part of 6- bromomethyl -3,4- dihydro -2- methyl-quinazoline -4- ketone, 100
Part liquefied ammonia, mixes 5h.
（2）Synthetic reaction
By weight, 100 parts of diammonium hydrogen phosphates and 110 parts of phosphorus pentoxides, 20 parts of urea, 4 parts of dodecanamide propyl sulfo group sweet teas
Dish alkali, 20 portions of ammonia buffer solutions carry out synthetic reaction, and product dries using filter, washing, crushes, both obtained II type ammonium polyphosphate
Fire proofing.Product identification M-3.
Comparative example 1：Lithium nitrate buffer solution is added without, the other the same as in Example 1.Products obtained therefrom number is M-4.
Comparative example 2：6- bromomethyl -3,4- dihydro -2- methyl-quinazoline -4- ketone is added without, the other the same as in Example 1.Institute
It is M-5 to obtain product identification.
Comparative example 3：Dodecanamide propyl sulfobetaines is added without, the other the same as in Example 1.Products obtained therefrom number is M-6.
Comparative example 4：
Ammonia buffer solution is added without, the other the same as in Example 1.Products obtained therefrom number is M-7.
Embodiment 4：
The ammonium polyphosphate of embodiment 1-3 and comparative example 1-4 will be added in, the degree of polymerization is detected to by HG/T2770-1996.
The comparison for the test specimen degree of polymerization that 1 different process of table is made.
| Number | The degree of polymerization |
| M-1 | 1756 |
| M-2 | 1717 |
| M-3 | 1856 |
| M-4 | 1112 |
| M-5 | 1156 |
| M-6 | 1180 |
| M-7 | 885 |
Claims (4)
1. a kind of preparation method of II type ammonium polyphosphate fire proofing, it is characterised in that step includes：
By weight, 100 parts of diammonium hydrogen phosphates and 80-110 parts of phosphorus pentoxides, 5-20 parts of urea, 1-4 parts of dodecanamide propyls
Sulfobetaines, 5-20 portions of ammonia buffer solutions carry out synthetic reaction, and product dries using filter, washing, crushes, both obtained II type
Ammonium polyphosphate fire proofing.
A kind of 2. preparation method of II type ammonium polyphosphate fire proofing described in claim 1, it is characterised in that synthetic reaction temperature
250~320 DEG C of degree.
3. the preparation method of a kind of II type ammonium polyphosphate fire proofing described in claim 1, it is characterised in that during synthetic reaction
Between 1-5h.
A kind of 4. preparation method of II type ammonium polyphosphate fire proofing described in claim 1, it is characterised in that the ammonia buffering
The preparation method of liquid includes：By weight, 0.1-0.5 portions of lithium nitrate buffer solutions, 0.01-0.1 parts of 6- bromomethyls -3,4- dihydros -
2- methyl-quinazoline -4- ketone, 100 parts of liquefied ammonia mix 1-5h.
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| CN201711199157.1A CN108059141A (en) | 2017-11-26 | 2017-11-26 | A kind of preparation method of II type ammonium polyphosphate fire proofing |
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| CN201711199157.1A CN108059141A (en) | 2017-11-26 | 2017-11-26 | A kind of preparation method of II type ammonium polyphosphate fire proofing |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994873A (en) * | 2006-12-28 | 2007-07-11 | 四川大学 | Ammonium polyphosphate continuous production method |
| CN101439851A (en) * | 2007-11-19 | 2009-05-27 | 北京理工大学 | Preparation of crystal type II ammonium polyphosphate |
| CN102585355A (en) * | 2011-12-23 | 2012-07-18 | 佛山佛塑科技集团股份有限公司 | Dispersing method of halogen-free flame retardant polypropylene |
| CN106586997A (en) * | 2016-12-16 | 2017-04-26 | 衢州普信新材料有限公司 | Preparation method of type II ammonium polyphosphate |
-
2017
- 2017-11-26 CN CN201711199157.1A patent/CN108059141A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994873A (en) * | 2006-12-28 | 2007-07-11 | 四川大学 | Ammonium polyphosphate continuous production method |
| CN101439851A (en) * | 2007-11-19 | 2009-05-27 | 北京理工大学 | Preparation of crystal type II ammonium polyphosphate |
| CN102585355A (en) * | 2011-12-23 | 2012-07-18 | 佛山佛塑科技集团股份有限公司 | Dispersing method of halogen-free flame retardant polypropylene |
| CN106586997A (en) * | 2016-12-16 | 2017-04-26 | 衢州普信新材料有限公司 | Preparation method of type II ammonium polyphosphate |
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