CN117551048A - Preparation method of efficient flame retardant dicyandiamide pyrophosphate salt - Google Patents
Preparation method of efficient flame retardant dicyandiamide pyrophosphate salt Download PDFInfo
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- CN117551048A CN117551048A CN202311419035.4A CN202311419035A CN117551048A CN 117551048 A CN117551048 A CN 117551048A CN 202311419035 A CN202311419035 A CN 202311419035A CN 117551048 A CN117551048 A CN 117551048A
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- pyrophosphoric acid
- water
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- melamine
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 34
- -1 flame retardant dicyandiamide pyrophosphate salt Chemical class 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 37
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229940005657 pyrophosphoric acid Drugs 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 17
- 230000035484 reaction time Effects 0.000 claims abstract description 11
- CZQYVJUCYIRDFR-UHFFFAOYSA-N phosphono dihydrogen phosphate;1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N)=N1.NC1=NC(N)=NC(N)=N1.OP(O)(=O)OP(O)(O)=O CZQYVJUCYIRDFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000010902 jet-milling Methods 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 11
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 9
- 239000011574 phosphorus Substances 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 238000005979 thermal decomposition reaction Methods 0.000 abstract description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 abstract description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 20
- 239000002994 raw material Substances 0.000 description 16
- 239000000047 product Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000000779 smoke Substances 0.000 description 6
- 235000011180 diphosphates Nutrition 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229940048084 pyrophosphate Drugs 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 4
- 229920000388 Polyphosphate Polymers 0.000 description 3
- 239000001205 polyphosphate Substances 0.000 description 3
- 235000011176 polyphosphates Nutrition 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 101710140186 Xaa-Pro aminopeptidase Proteins 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/40—Nitrogen atoms
- C07D251/54—Three nitrogen atoms
- C07D251/56—Preparation of melamine
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention discloses a preparation method of efficient flame retardant dicyandiamide pyrophosphate salt, which comprises the following steps of; 1) Adding pyrophosphoric acid and part of water into a reaction kettle for mixing and dissolving, 2) adding melamine and the rest water into the reaction kettle after mixing, wherein the reaction time is 3-5 h, and the material is heated to 12-16 ℃ due to the exothermic process in the reaction process; 3) After the reaction is finished, the materials are centrifugated, dried and crushed to finally obtain the dimelamine pyrophosphate product. The invention adopts solid phosphorus source, and overcomes the defect that the common liquid phosphoric acid is difficult to transport and store. In addition, the synthesis process is simple to operate, mild in condition, free of catalyst, easy to separate and adopts water as a solvent. In addition, the reaction process is stable and controllable, the time is short, the energy consumption is low, and the method is environment-friendly. The physicochemical property and thermal decomposition property of the product are analyzed and compared, and the product of the invention is excellent.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to a preparation method of efficient flame retardant dicyandiamide pyrophosphate salt.
Background
The traditional halogen flame retardant has excellent flame retardant effect and is a flame retardant material widely applied at present, but the flame retardant has large smoke quantity, is poisonous and has corrosive gas during combustion, and has great harm, so that the human health is seriously influenced, the ecology is destroyed and the environment is polluted to a great extent. In recent years, with the increasing awareness of environmental protection, halogen flame retardants have been replaced with environmentally friendly phosphorus flame retardants. The phosphorus flame retardant has the advantages of low smoke, low toxicity, no halogen, environmental friendliness and the like, is mainly flame-retardant by condensed phase, forms a mass and heat transfer barrier on the surface of a material during thermal cracking or combustion, has less smoke generation amount, toxic and corrosive gas generation amount in the flame retardant process, has production degradation characteristics, and can not encounter the problems of environmental persistence and biological accumulation in the use process.
The dicyandiamide pyrophosphate (Dimelamine pyrophosphate, DMPY) is white crystal powder as a nitrogen-phosphorus intumescent flame retardant, has higher nitrogen content and nitrogen-phosphorus synergistic effect, has the characteristics of good thermal stability, excellent flame retardant property, good compatibility with a base material, environmental protection, no halogen, low smoke, water resistance and the like, is an ideal substitute product of APP-II type, and is mainly used in polyolefin, paint, wood, fiber and the like. To date, the synthesis process of the melamine polyphosphate flame retardant is in a preliminary exploration stage in domestic and foreign researches, and has few patent reports, and the synthesis process mainly comprises the following steps: (1) The process has the advantages that phosphorus pentoxide and melamine are used as raw materials to synthesize the dimelamine pyrophosphate, and the phosphorus pentoxide is extremely easy to absorb moisture and difficult to store. (2) The method is characterized in that melamine, nitric acid and sodium pyrophosphate are used as raw materials, the melamine and water are firstly mixed, the temperature is raised to 80 ℃ for stirring, and then sodium pyrophosphate is added for continuous reaction, so that the dimelamine pyrophosphate is finally synthesized. The process uses strong acid, has dangers, has higher reaction temperature and consumes energy; sodium nitrate by-product is produced at the same time, and the removing procedure is added. In view of the above problems, there is an urgent need for a method for preparing a flame retardant with high efficiency.
Disclosure of Invention
The invention provides a preparation method of efficient flame retardant dicyandiamide pyrophosphate.
The scheme of the invention is as follows:
a preparation method of efficient flame retardant dicyandiamide pyrophosphate salt comprises the following steps:
1) The pyrophosphoric acid and melamine are weighed, the pyrophosphoric acid serving as a raw material is used as a solid phosphorus source, the defect that a common liquid phosphorus source is difficult to transport and store is overcome, and the raw material is extremely easy to absorb moisture and decompose and needs to be stored in a sealing way; the melamine as a raw material is a polymer with high nitrogen content, high flame retardant efficiency, low smoke and toxicity and good thermal stability, and can be singly used as a flame retardant or reacted with other substances to synthesize the flame retardant; firstly adding part of water into a reaction kettle, and then slowly adding pyrophosphoric acid into the water for dissolution, wherein the stirring speed is 25Hz;
2) Mixing melamine with the residual water, and then adding the mixture into a reaction kettle, wherein the stirring speed is 50Hz; the reaction time is 3-5 h, the reaction process is an exothermic process, the temperature of the materials is raised to 12-16 ℃, and meanwhile, sampling analysis is carried out per hour;
3) After the reaction is finished, centrifuging, drying and crushing the materials to finally obtain a dimelamine pyrophosphate product;
the reaction formula is as follows:
as a preferred technical scheme, the molar ratio of the pyrophosphoric acid to the melamine is 1:1.75 to 2.25.
As a preferable technical scheme, the water addition amount is 6-8 times of the sum of the masses of the pyrophosphoric acid and the melamine.
As a preferable technical scheme, the 1) part of water is 4.6 times of the sum of the masses of pyrophosphoric acid and melamine; the residual water in the step 2) is 2.4 times of the sum of the masses of the pyrophosphoric acid and the melamine.
As a preferable technical scheme, the reaction time is 3-5 h, the cooling temperature is 0 ℃, the reaction is an exothermic process, and the temperature of materials is raised to 15 ℃.
As a preferable technical scheme, after the reaction of 3), carrying out solid-liquid separation on the materials by a centrifugal machine, temporarily storing centrifugal liquid, taking out the solid, and returning the solid to a reaction kettle for water washing, wherein the washing water quantity is 1-2 times of the total materials; and (3) centrifuging again, drying the solid in an oven at 120 ℃ for 24 hours, and jet milling.
In order to avoid the problem of agglomeration caused by direct addition of melamine.
When the pyrophosphoric acid is added into water, the stirring speed is 25Hz, so that the reaction is prevented from being too fast, the temperature is increased, and the pyrophosphoric acid is decomposed; and then, when the melamine and water are mixed and added into the reaction kettle, the stirring speed is 50Hz, the materials are prevented from caking, and the reaction can be accelerated.
The reaction time is 4 hours, the reaction process is an exothermic process, the temperature of the materials is raised to 15 ℃, and meanwhile, sampling analysis is carried out per hour, and the N, P content and the pH condition of the reaction process are observed.
Due to the adoption of the technical scheme, the preparation method of the efficient flame retardant dicyandiamide pyrophosphate comprises the following steps of: 1) The pyrophosphoric acid and melamine are weighed, the pyrophosphoric acid serving as a raw material is used as a solid phosphorus source, the defect that a common liquid phosphorus source is difficult to transport and store is overcome, and the raw material is extremely easy to absorb moisture and decompose and needs to be stored in a sealing way; the melamine as a raw material is a polymer with high nitrogen content, high flame retardant efficiency, low smoke and toxicity and good thermal stability, and can be singly used as a flame retardant or reacted with other substances to synthesize the flame retardant; setting the temperature of a mold temperature machine to be 0 ℃, adding part of water into a kneader, and then slowly adding pyrophosphoric acid into the water for dissolution, wherein the stirring speed is 25Hz; 2) Mixing melamine with the residual water, and then adding the mixture into a reaction kettle, wherein the stirring speed is 50Hz; the reaction time is 3-5 h, the reaction process is an exothermic process, the temperature of the materials is raised to 12-16 ℃, and meanwhile, sampling analysis is carried out per hour; 3) After the reaction is finished, the materials are centrifugated, dried and crushed to finally obtain the dimelamine pyrophosphate product.
The invention has the advantages that:
the invention has simple process operation, mild reaction condition, simple acid-base neutralization reaction, no need of catalyst, water as solvent and easy centrifugal separation. In addition, the reaction process is stable and controllable, the time is short, the energy consumption is low, and the method is environment-friendly.
(1) The invention develops a synthesis process of melamine polyphosphate with high polymerization degree, adopts solid phosphorus source as raw materials, and overcomes the defect that common liquid phosphoric acid (serving as phosphorus source) is difficult to transport and store.
(2) The synthesis process is simple, the reaction condition is mild, and the method is a simple acid-base neutralization reaction, and no catalyst is needed.
(3) The reaction process is stable and controllable, the time is short, the energy consumption is low, the environmental pollution is small, water is used as a solvent, and the centrifugal separation is easy.
(4) The raw materials are abundant in source, low in cost and easy for industrial production.
Detailed Description
The invention provides a preparation method of efficient flame retardant dicyandiamide pyrophosphate.
The invention is further described in connection with the following embodiments in order to make the technical means, the creation features, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
Taking pyrophosphoric acid and melamine as raw materials, weighing the raw materials in a molar ratio of 1:1.75, setting the temperature of a mold temperature machine to be 0 ℃, adding part of water (4.6 times of the sum of the mass of pyrophosphoric acid and the mass of melamine) into a kneader, slowly adding pyrophosphoric acid into the water for dissolution, and stirring at a speed of 25Hz. Finally, mixing melamine with the residual water (2.4 times of the sum of the masses of the pyrophosphoric acid and the melamine), and adding the mixture into a reaction kettle, wherein the stirring speed is 50Hz. The reaction time was 3h, and the material was warmed to 12℃as the reaction process was exothermic, and samples were taken and analyzed per hour. After the reaction is finished, centrifuging, drying and crushing the materials to finally obtain the dimelamine pyrophosphate product, wherein the product detection indexes are shown in table 1.
Example 2
Taking pyrophosphoric acid and melamine as raw materials, weighing the raw materials in a molar ratio of 1:2, setting the temperature of a mold temperature machine to be 0 ℃, adding part of water (4.6 times of the sum of the mass of pyrophosphoric acid and melamine) into a kneader, slowly adding pyrophosphoric acid into the water for dissolution, and stirring at a speed of 25Hz. Finally, mixing melamine with the residual water (2.4 times of the sum of the masses of the pyrophosphoric acid and the melamine), and adding the mixture into a reaction kettle, wherein the stirring speed is 50Hz. The reaction time was 4h, and the material was warmed to 15℃as the reaction process was exothermic, and samples were taken and analyzed per hour. After the reaction is finished, centrifuging, drying and crushing the materials to finally obtain the dimelamine pyrophosphate product, wherein the product detection indexes are shown in table 1.
Example 3
Taking pyrophosphoric acid and melamine as raw materials, weighing the raw materials in a molar ratio of 1:2.25, setting the temperature of a mold temperature machine to be 0 ℃, adding part of water (4.6 times of the sum of the mass of pyrophosphoric acid and the mass of melamine) into a kneader, slowly adding pyrophosphoric acid into the water for dissolution, and stirring at a speed of 25Hz. Finally, mixing melamine with the residual water (2.4 times of the sum of the masses of the pyrophosphoric acid and the melamine), and adding the mixture into a reaction kettle, wherein the stirring speed is 50Hz. The reaction time was 5h, and the material was warmed to 16℃as the reaction process was exothermic, and samples were taken and analyzed per hour. After the reaction is finished, centrifuging, drying and crushing the materials to finally obtain the dimelamine pyrophosphate product, wherein the product detection indexes are shown in table 1.
TABLE 1 detection index of melamine polyphosphate product
| Index (I) | Commercially available | Example 1 | Example 2 | Example 3 |
| N(％) | ≥38％ | 38.83 | 39.27 | 39.51 |
| P 2 O 5 (％) | ≥32％ | 34.12 | 33.72 | 33.66 |
| pH(10g/L) | 3.8±0.5 | 3.79 | 3.83 | 3.89 |
| 1% thermal decomposition temperature (. Degree. C.) | ≥260 | 267 | 271 | 268 |
| 5% thermal decomposition temperature (. Degree. C.) | ≥300 | 307 | 310 | 305 |
The product indexes in the embodiment all meet the requirements, and have higher N, P content and higher decomposition temperature. In addition, for the present invention, the synthesis process of example 2 was optimal, i.e., the molar ratio of pyrophosphate to melamine was 1:2, the cooling temperature was 0 ℃, the feed temperature was about 15 ℃, and the reaction time was 4h.
The foregoing has shown and described the basic principles, main features and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The preparation method of the efficient flame retardant dicyandiamide pyrophosphate salt is characterized by comprising the following steps of:
1) Firstly, adding part of water into a reaction kettle, and then slowly adding pyrophosphoric acid into the water for dissolution, wherein the stirring rate is 25Hz;
2) Mixing melamine with the residual water, and then adding the mixture into a reaction kettle, wherein the stirring speed is 50Hz; the reaction time is 3-5 h, the reaction process is an exothermic process, the temperature of the materials is raised to 12-16 ℃, and meanwhile, sampling analysis is carried out per hour;
3) After the reaction is finished, centrifuging, drying and crushing the materials to finally obtain a dimelamine pyrophosphate product;
the reaction formula is as follows:
2. the method for preparing the efficient flame retardant dicyandiamide salt of pyrophosphoric acid as claimed in claim 1, which is characterized in that: the molar ratio of the pyrophosphoric acid to the melamine is 1:1.75 to 2.25.
3. The method for preparing the efficient flame retardant dicyandiamide salt of pyrophosphoric acid as claimed in claim 1, which is characterized in that: the water addition amount is 6-8 times of the sum of the masses of the pyrophosphoric acid and the melamine.
4. The method for preparing the efficient flame retardant dicyandiamide salt of pyrophosphoric acid as claimed in claim 1, which is characterized in that: the partial water in the step 1) is 4.6 times of the sum of the masses of the pyrophosphoric acid and the melamine; the residual water in the step 2) is 2.4 times of the sum of the masses of the pyrophosphoric acid and the melamine.
5. The method for preparing the efficient flame retardant dicyandiamide salt of pyrophosphoric acid as claimed in claim 1, which is characterized in that: the reaction time is 3-5 h, the cooling temperature is 0 ℃, the reaction is an exothermic process, and the temperature of the materials is raised to 15 ℃.
6. The method for preparing the efficient flame retardant dicyandiamide salt of pyrophosphoric acid as claimed in claim 1, which is characterized in that: after the reaction of 3), carrying out solid-liquid separation on the materials by a centrifugal machine, temporarily storing the centrifugate, taking out the solid, and returning the solid to a reaction kettle for water washing, wherein the washing water amount is 1-2 times of the total materials; and (3) centrifuging again, drying the solid in an oven at 120 ℃ for 24 hours, and jet milling.
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