CN112480166A - Preparation method of nitrogen-phosphorus flame retardant - Google Patents
Preparation method of nitrogen-phosphorus flame retardant Download PDFInfo
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- CN112480166A CN112480166A CN202011371433.XA CN202011371433A CN112480166A CN 112480166 A CN112480166 A CN 112480166A CN 202011371433 A CN202011371433 A CN 202011371433A CN 112480166 A CN112480166 A CN 112480166A
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- flame retardant
- nitrogen
- phosphorus flame
- phosphate
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 52
- 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 title claims abstract description 49
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 11
- 239000010452 phosphate Substances 0.000 claims abstract description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 6
- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 claims description 5
- VONWDASPFIQPDY-UHFFFAOYSA-N dimethyl methylphosphonate Chemical compound COP(C)(=O)OC VONWDASPFIQPDY-UHFFFAOYSA-N 0.000 claims description 5
- BDZBKCUKTQZUTL-UHFFFAOYSA-N triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 claims description 5
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 4
- 150000007519 polyprotic acids Polymers 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- AATNZNJRDOVKDD-UHFFFAOYSA-N 1-[ethoxy(ethyl)phosphoryl]oxyethane Chemical compound CCOP(=O)(CC)OCC AATNZNJRDOVKDD-UHFFFAOYSA-N 0.000 claims description 2
- CZHYKKAKFWLGJO-UHFFFAOYSA-N dimethyl phosphite Chemical compound COP([O-])OC CZHYKKAKFWLGJO-UHFFFAOYSA-N 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 2
- -1 phosphate ester Chemical class 0.000 claims 1
- 229920000728 polyester Polymers 0.000 abstract description 5
- 229920004933 Terylene® Polymers 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 4
- 230000026030 halogenation Effects 0.000 abstract description 3
- 238000005658 halogenation reaction Methods 0.000 abstract description 3
- 230000000979 retarding effect Effects 0.000 abstract description 3
- 229920000742 Cotton Polymers 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000006378 damage Effects 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/141—Esters of phosphorous acids
- C07F9/1411—Esters of phosphorous acids with hydroxyalkyl compounds with further substituents on alkyl
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/091—Esters of phosphoric acids with hydroxyalkyl compounds with further substituents on alkyl
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/40—Esters thereof
- C07F9/4071—Esters thereof the ester moiety containing a substituent or a structure which is considered as characteristic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus
- D06M13/447—Phosphonates or phosphinates containing nitrogen atoms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus
- D06M13/453—Phosphates or phosphites containing nitrogen atoms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Fireproofing Substances (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method of a nitrogen-phosphorus flame retardant, which comprises the steps of mixing triethanolamine and phosphate according to a proportion, adding a catalyst, and reacting for 3-20 hours at the temperature of 60-180 ℃ to prepare the novel nitrogen-phosphorus flame retardant. Compared with the prior art, the nitrogen-phosphorus flame retardant disclosed by the invention completely realizes no halogenation, can be used for flame retarding of materials such as terylene and polyester cotton, and has a good flame retarding effect; and has the advantages of simple process and high reaction efficiency.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to a preparation method of a nitrogen-phosphorus flame retardant.
Background
The textile has the characteristic of inflammability, is easy to cause fire in the using process, and can greatly reduce the probability of fire when being subjected to flame retardant finishing. The halogen flame retardant is a flame retardant which is used more, but because of the problem of environmental pollution and the harm of dioxin to human bodies, the use of halogen-containing flame retardant products is prohibited internationally. Under the drive of non-halogenation, the phosphorus-containing flame retardant and the nitrogen-phosphorus flame retardant meet the requirements of environmental protection, good compatibility with matrix materials, high flame retardant efficiency and the like, and become the current development trend. The nitrogen element is added into the phosphorus-containing flame retardant, and the defects of high volatility, poor compatibility, poor heat resistance, dripping and the like of the phosphorus-containing flame retardant are overcome through N, P synergistic effect on the basis of the existing phosphorus-containing flame retardant, so that the flame retardant efficiency is improved, and the flame retardant effect is enhanced. How to further improve the flame retardant efficiency of the nitrogen-phosphorus flame retardant becomes the key point of research.
Disclosure of Invention
The invention aims to overcome the defects of complex preparation process and poor flame retardant effect in the prior art, and provides a preparation method of a nitrogen-phosphorus flame retardant, so as to enhance the flame retardant effect and improve the flame retardant efficiency.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a nitrogen-phosphorus flame retardant comprises the following specific steps: mixing triethanolamine and phosphate, adding a catalyst, and reacting at 60-180 ℃ for 3-20h to obtain the nitrogen-phosphorus flame retardant.
The molar ratio of the triethanolamine to the phosphate is 1: 1.05-1: 1.5.
Preferably, the molar ratio of the triethanolamine to the phosphate is 1: 1.05-1: 1.3.
The phosphate is selected from one or more of dimethyl methylphosphonate, diethyl ethylphosphonate, trimethyl phosphate, triethyl phosphate, dimethyl phosphite, diethyl phosphite, trimethyl phosphite or triethyl phosphite. Preferably, the phosphate is selected from one of triethyl phosphite, dimethyl methyl phosphonate, trimethyl phosphate and diethyl phosphite.
The catalyst is polybasic acid or polybasic base.
The polybasic acid is selected from one or more of p-toluenesulfonic acid, concentrated sulfuric acid, hydrochloric acid or acetic acid;
the polybasic alkali is selected from one or more of triethylamine, sodium methoxide, sodium ethoxide, potassium hydroxide, potassium carbonate or sodium carbonate.
The dosage of the catalyst is 0.1-6% of the weight of the triethanolamine.
Preferably, the amount of the catalyst is 1-4% of the weight of the triethanolamine.
Compared with the prior art, the invention has the following advantages:
(1) the nitrogen-phosphorus flame retardant has good flame retardant effect, can greatly shorten the afterflame time and reduce the damage length of the polyester fabric when being used for the polyester fabric, and the burnt fabric has no molten drops;
(2) the nitrogen-phosphorus flame retardant disclosed by the invention completely realizes no halogenation, can be used for flame retardance of materials such as terylene and polyester cotton, and has a good flame retardant effect;
(3) the whole preparation process is simple, the flame retardant is obtained by one-step reaction, the reaction efficiency is high, and the production is easy to expand.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
Mixing 29.8g of triethanolamine and 34.89g of triethyl phosphite, adding 0.97g of p-toluenesulfonic acid, introducing nitrogen for protection, reacting at 85 ℃ for 6 hours, carrying out reduced pressure distillation to remove unreacted raw materials and byproducts, and cooling to obtain a white sticky solid, namely the novel nitrogen-phosphorus flame retardant.
The thick solid is the novel nitrogen-phosphorus flame retardant.
Example 2
33.15g of triethanolamine and 39.78g of dimethyl methylphosphonate are mixed, 1.46g of concentrated sulfuric acid is added, nitrogen is introduced for protection, the mixture reacts for 6 hours at the temperature of 150 ℃, unreacted raw materials and byproducts are removed by reduced pressure distillation, and white sticky solid, namely the novel nitrogen-phosphorus flame retardant, is obtained after cooling.
Example 3
37.30g of triethanolamine and 44.74g of trimethyl phosphate are mixed, 1.64g of triethylamine is added, nitrogen is introduced for protection, the mixture reacts for 7 hours at 95 ℃, unreacted raw materials and byproducts are removed by reduced pressure distillation, and white sticky solid, namely the novel nitrogen-phosphorus flame retardant, is obtained after cooling.
Example 4
Mixing 42.63g of triethanolamine and 56.97g of diethyl phosphite, adding 2.48g of potassium hydroxide, introducing nitrogen for protection, reacting at 75 ℃ for 5 hours, carrying out reduced pressure distillation to remove unreacted raw materials and byproducts, and cooling to obtain a white sticky solid, namely the novel nitrogen-phosphorus flame retardant.
Example 5
In this example, for evaluation example, the novel nitrogen-phosphorus flame retardant prepared in examples 1 to 4 was finished with 30 wt% of flame retardant at a baking temperature of 180 ℃ for 120s of baking time to obtain finished samples 1 to 4, respectively, and the flame retardant effect is shown in table 1 by using polyester without added flame retardant as a control.
TABLE 1 evaluation of flame retarding Effect of flame retardants
| Flame retardant | Time of continuous combustion(s) | Smoldering time(s) | Length of damage (mm) | Molten drop |
| Terylene | 15 | 0 | 150 | Is provided with |
| Finishing sample 1 | 0 | 0 | 15 | Is free of |
| Preparation of sample 2 | 0 | 0 | 20 | Is free of |
| Arrangement of samples 3 | 2 | 0 | 25 | Is rarely used |
| Finishing sample 4 | 3 | 0 | 30 | Small amount of |
As can be seen from Table 1, the afterflame time of the terylene treated by the flame retardant is greatly reduced, the damage length is also greatly reduced, and no molten drop phenomenon or only a very small amount of molten drops appear in the combustion process. This shows that the flame retardants of examples 1 to 5 have excellent flame retardant effect.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A preparation method of a nitrogen-phosphorus flame retardant is characterized in that triethanolamine and phosphate are mixed and then added with a catalyst to react for 3-20 hours at the temperature of 60-180 ℃ to obtain the nitrogen-phosphorus flame retardant.
2. The preparation method of the nitrogen-phosphorus flame retardant according to claim 1, wherein the molar ratio of the triethanolamine to the phosphate is 1:1.05 to 1: 1.5.
3. The preparation method of the nitrogen-phosphorus flame retardant according to claim 2, wherein the molar ratio of the triethanolamine to the phosphate is 1:1.05 to 1: 1.3.
4. The method as claimed in claim 1, wherein the phosphate is one or more selected from dimethyl methylphosphonate, diethyl ethylphosphonate, trimethyl phosphate, triethyl phosphate, dimethyl phosphite, diethyl phosphite, trimethyl phosphite and triethyl phosphite.
5. The method of claim 4, wherein the phosphate ester is selected from triethyl phosphite, dimethyl methylphosphonate, trimethyl phosphate, and diethyl phosphite.
6. The method according to claim 1, wherein the catalyst is a polybasic acid or a polybasic base.
7. The method according to claim 6, wherein the polybasic acid is selected from one or more of p-toluenesulfonic acid, concentrated sulfuric acid, hydrochloric acid or acetic acid.
8. The method according to claim 6, wherein the polybasic base is one or more selected from triethylamine, sodium methoxide, sodium ethoxide, potassium hydroxide, potassium carbonate and sodium carbonate.
9. The preparation method of the nitrogen-phosphorus flame retardant as claimed in claim 1, wherein the amount of the catalyst is 0.1-6% of the mass of the triethanolamine.
10. The method for preparing nitrogen-phosphorus flame retardant according to claim 9, wherein the amount of the catalyst is 1-4% of the weight of triethanolamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202011371433.XA CN112480166A (en) | 2020-11-30 | 2020-11-30 | Preparation method of nitrogen-phosphorus flame retardant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011371433.XA CN112480166A (en) | 2020-11-30 | 2020-11-30 | Preparation method of nitrogen-phosphorus flame retardant |
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| CN112480166A true CN112480166A (en) | 2021-03-12 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114752298A (en) * | 2022-03-31 | 2022-07-15 | 山东天盾矿用设备有限公司 | Embedded channel sealing coating and preparation method and application thereof |
| CN115028792A (en) * | 2022-07-04 | 2022-09-09 | 上海应用技术大学 | Hyperbranched phosphorus-bromine synergistic polyurethane flame retardant and preparation method thereof |
| CN117364487A (en) * | 2023-12-04 | 2024-01-09 | 江苏恒力化纤股份有限公司 | Preparation method of durable flame-retardant coating polyester/cotton blended fabric |
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- 2020-11-30 CN CN202011371433.XA patent/CN112480166A/en active Pending
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114752298A (en) * | 2022-03-31 | 2022-07-15 | 山东天盾矿用设备有限公司 | Embedded channel sealing coating and preparation method and application thereof |
| CN115028792A (en) * | 2022-07-04 | 2022-09-09 | 上海应用技术大学 | Hyperbranched phosphorus-bromine synergistic polyurethane flame retardant and preparation method thereof |
| CN115028792B (en) * | 2022-07-04 | 2023-09-26 | 上海应用技术大学 | Hyperbranched phosphorus-bromine synergistic polyurethane flame retardant and preparation method thereof |
| CN117364487A (en) * | 2023-12-04 | 2024-01-09 | 江苏恒力化纤股份有限公司 | Preparation method of durable flame-retardant coating polyester/cotton blended fabric |
| CN117364487B (en) * | 2023-12-04 | 2024-03-19 | 江苏恒力化纤股份有限公司 | Preparation method of durable flame-retardant coating polyester/cotton blended fabric |
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Application publication date: 20210312 |