CN112159669A - Preparation method of phosphorus-containing macromolecular intumescent flame-retardant char-forming agent - Google Patents
Preparation method of phosphorus-containing macromolecular intumescent flame-retardant char-forming agent Download PDFInfo
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- 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 27
- 239000003063 flame retardant Substances 0.000 title claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 14
- 239000011574 phosphorus Substances 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 72
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims abstract description 12
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 30
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 18
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 18
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 15
- 239000012295 chemical reaction liquid Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910019142 PO4 Inorganic materials 0.000 claims description 7
- 239000010452 phosphate Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000006467 substitution reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 125000001309 chloro group Chemical group Cl* 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 150000003918 triazines Chemical class 0.000 abstract description 2
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 239000002131 composite material Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 150000005846 sugar alcohols Polymers 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000010000 carbonizing Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- -1 phosphate ester Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
- C09K21/06—Organic materials
- C09K21/12—Organic materials containing phosphorus
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- 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
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6558—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing at least two different or differently substituted hetero rings neither condensed among themselves nor condensed with a common carbocyclic ring or ring system
- C07F9/65583—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom containing at least two different or differently substituted hetero rings neither condensed among themselves nor condensed with a common carbocyclic ring or ring system each of the hetero rings containing nitrogen as ring hetero atom
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
- C08G79/04—Phosphorus linked to oxygen or to oxygen and carbon
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/14—Macromolecular materials
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Abstract
The invention discloses a preparation method of a phosphorus-containing macromolecular intumescent flame-retardant char-forming agent, which belongs to the technical field of flame-retardant char-forming agent preparation, adopts triazine derivatives which have tertiary oxygen structures and stable triazine ring structures, have good char-forming capability and thermal stability, can effectively improve the water resistance and flame-retardant property of materials, adopts cyanuric chloride for substitution reaction, has high chlorine atom activity on the cyanuric chloride, is easy to carry out affinity substitution reaction, is beneficial to constructing compounds with flame-retardant function, replaces chlorine atoms with different reaction activities at different temperatures, obtains reactants with different purposes and properties by controlling the temperature process, adopts cyanuric chloride, polyhydric alcohol and piperazine as raw materials, synthesizes a char-forming agent by substitution reaction, has outstanding thermal stability, char-forming property and thermal stability simultaneously, The flame retardant has good combustibility and water resistance, and can be well used in different composite materials.
Description
Technical Field
The invention relates to the technical field of preparation of flame-retardant charring agents, in particular to a preparation method of a phosphorus-containing macromolecular intumescent flame-retardant charring agent.
Background
The intumescent flame retardant is free of halogen, an intumescent carbon layer is formed in the combustion process, the intumescent flame retardant has the functions of oxygen isolation, heat insulation, drip prevention, smoke suppression and the like for the interior, and is a green and environment-friendly flame retardant. Namely an acid source, a carbon source and a gas source. The existing carbonizing agent is prepared by compounding ammonium polyphosphate, pentaerythritol and melamine in the field of preparing carbonizing agents, and the existing carbonizing agent formed by taking the ammonium polyphosphate as a basic system has the defects of easy migration and reaction with the ammonium polyphosphate in the processing process to generate phosphate ester, and can play a flame retardant effect only by depending on the ammonium polyphosphate, and the flame retardant performance of the carbonizing agent can be influenced due to the characteristics of the ammonium polyphosphate.
Disclosure of Invention
The invention aims to provide a preparation method of a phosphorus-containing macromolecular intumescent flame-retardant charring agent, which aims to solve the problems that the phosphorus-containing macromolecular intumescent flame-retardant charring agent is easy to migrate and can react with ammonium polyphosphate in the processing process to generate phosphate in the background art, the flame-retardant effect can be exerted only by a large amount of ammonium polyphosphate, and the flame-retardant property of the charring agent is influenced by the characteristics of the ammonium polyphosphate.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a phosphorus-containing macromolecular intumescent flame-retardant char-forming agent comprises the following steps:
step 1: pouring cyanuric chloride and ethylenediamine into a bottle, stirring and dissolving to obtain a first solution, stirring the first solution, dropwise adding a second solution into the first solution while stirring, after dropwise adding for more than one hour, injecting nitrogen into the bottle, and reacting the first solution and the second solution for 3 hours under the nitrogen maintenance condition to obtain a first reaction solution, wherein the reaction temperature is 10-15 ℃;
step 2: dropwise adding the solution III into the first reaction solution reacted in the step 1, and stirring the first reaction solution to ensure that the first reaction solution and the solution III are fully reacted to obtain a second reaction solution, wherein the reaction temperature is 50-80 ℃, and the reaction time is 3 hours;
and step 3: dropwise adding the other part of the solution III into the second reaction solution reacted in the step 2, stirring the second reaction solution to enable the second reaction solution and the solution III to fully react, and fully reacting at the reflux temperature for 6-8 hours to obtain a third reaction solution;
and 4, step 4: and (3) cooling the third reaction liquid in the step (3) to room temperature, filtering and washing the third reaction liquid for multiple times by using water and ethanol, adding ammonium polyphosphate into the third reaction liquid, uniformly stirring, and drying in an oven to obtain a finished product, wherein the temperature is 80-110 ℃, and the time is 24 hours.
Preferably, the second solution in the step 1 comprises ethanolamine, alcohol phosphate and triethylamine, and the molar ratio of the second solution to the first solution is 1: 2-5.
Preferably, the solution three in the step 2 comprises ethanolamine, piperazine and sodium hydroxide, and the molar ratio of the solution three to the first reaction solution in the step 2 is 2: 1-2.
Preferably, the pH of the first reaction solution in the step 1 is 5 to 7.
Preferably, the pH of the second reaction solution in the step 2 is 5 to 7.
And in the step 4, the ammonium polyphosphate accounts for 20-30% of the finished product in percentage by weight.
Compared with the prior art, the invention has the beneficial effects that:
1) the triazine derivative has a tertiary oxygen structure and a stable triazine ring structure, has good char forming capability and thermal stability, and can effectively improve the water resistance and flame retardance of the material.
2) The method adopts cyanuric chloride to carry out substitution reaction, the activity of chlorine atoms on the cyanuric chloride is very high, the affinity substitution reaction is easy to carry out, and the method is favorable for constructing the compound with the flame retardant function.
Drawings
FIG. 1 is a schematic flow diagram of the present invention;
FIG. 2 is a graph showing the results of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
Referring to fig. 1, the present invention provides a technical solution:
example 1:
a preparation method of a phosphorus-containing macromolecular intumescent flame-retardant char-forming agent comprises the following steps:
step 1: pouring cyanuric chloride and ethylenediamine into a bottle, stirring and dissolving to obtain a first solution, stirring the first solution, dropwise adding a second solution into the first solution while stirring, after dropwise adding for more than one hour, injecting nitrogen into the bottle, and reacting the first solution and the second solution for 3 hours under the nitrogen maintenance condition to obtain a first reaction solution, wherein the reaction temperature is 10 ℃;
step 2: dropwise adding the solution III into the first reaction solution reacted in the step 1, and stirring the first reaction solution to ensure that the first reaction solution and the solution III are fully reacted to obtain a second reaction solution, wherein the reaction temperature is 50 ℃, and the reaction time is 3 hours;
and step 3: dropwise adding the other part of the solution III into the second reaction solution reacted in the step 2, stirring the second reaction solution to enable the second reaction solution and the solution III to fully react, and fully reacting for 6 hours at a reflux temperature to obtain a third reaction solution;
and 4, step 4: and (3) cooling the third reaction liquid in the step (3) to room temperature, filtering and washing the third reaction liquid for multiple times by using water and ethanol, adding ammonium polyphosphate into the third reaction liquid, uniformly stirring, and drying in an oven to obtain a finished product, wherein the temperature is 80 ℃ and the time is 24 hours.
The second solution in the step 1 comprises ethanolamine, alcohol phosphate and triethylamine, and the molar ratio of the second solution to the first solution is 1: 2.
The solution III in the step 2 comprises ethanolamine, piperazine and sodium hydroxide, and the molar ratio of the solution III to the first reaction solution in the step 2 is 2: 1.
the pH value of the first reaction solution in the step 1 is 5.
The pH value of the second reaction solution in the step 2 is 5.
And in the step 4, the ammonium polyphosphate accounts for 20 percent of the finished product in percentage by weight.
Example 2:
step 1: pouring cyanuric chloride and ethylenediamine into a bottle, stirring and dissolving to obtain a first solution, stirring the first solution, dropwise adding a second solution into the first solution while stirring, after dropwise adding for more than one hour, injecting nitrogen into the bottle, and reacting the first solution and the second solution for 3 hours under the nitrogen maintenance condition to obtain a first reaction solution, wherein the reaction temperature is 15 ℃;
step 2: dropwise adding the solution III into the first reaction solution reacted in the step 1, and stirring the first reaction solution to ensure that the first reaction solution and the solution III are fully reacted to obtain a second reaction solution, wherein the reaction temperature is 80 ℃, and the reaction time is 3 hours;
and step 3: dropwise adding the other part of the solution III into the second reaction solution reacted in the step 2, stirring the second reaction solution to enable the second reaction solution and the solution III to fully react, and fully reacting at the reflux temperature for 8 hours to obtain a third reaction solution;
and 4, step 4: and (3) cooling the third reaction liquid in the step (3) to room temperature, filtering and washing the third reaction liquid for multiple times by using water and ethanol, adding ammonium polyphosphate into the third reaction liquid, uniformly stirring, and drying in an oven to obtain a finished product, wherein the temperature is 110 ℃ and the time is 24 hours.
The second solution in the step 1 comprises ethanolamine, alcohol phosphate and triethylamine, and the molar ratio of the second solution to the first solution is 1: 2.
The solution III in the step 2 comprises ethanolamine, piperazine and sodium hydroxide, and the molar ratio of the solution III to the first reaction solution in the step 2 is 2: 1.
the pH value of the first reaction solution in the step 1 is 7.
The pH value of the second reaction solution in the step 2 is 7.
And in the step 4, the ammonium polyphosphate accounts for 20 percent of the finished product in percentage by weight.
Example 3:
step 1: pouring cyanuric chloride and ethylenediamine into a bottle, stirring and dissolving to obtain a first solution, stirring the first solution, dropwise adding a second solution into the first solution while stirring, after dropwise adding for more than one hour, injecting nitrogen into the bottle, and reacting the first solution and the second solution for 3 hours under the nitrogen maintenance condition to obtain a first reaction solution, wherein the reaction temperature is 10 ℃;
step 2: dropwise adding the solution III into the first reaction solution reacted in the step 1, and stirring the first reaction solution to ensure that the first reaction solution and the solution III are fully reacted to obtain a second reaction solution, wherein the reaction temperature is 60 ℃, and the reaction time is 3 hours;
and step 3: dropwise adding the other part of the solution III into the second reaction solution reacted in the step 2, stirring the second reaction solution to enable the second reaction solution and the solution III to fully react, and fully reacting at the reflux temperature for 8 hours to obtain a third reaction solution;
and 4, step 4: and (3) cooling the third reaction liquid in the step (3) to room temperature, filtering and washing the third reaction liquid for multiple times by using water and ethanol, adding ammonium polyphosphate into the third reaction liquid, uniformly stirring, and drying in an oven to obtain a finished product, wherein the temperature is 90 ℃ and the time is 24 hours.
Wherein the solution II in the step 1 comprises ethanolamine, alcohol phosphate and triethylamine, and the molar ratio of the solution II to the solution I is 1: 5.
The solution III in the step 2 comprises ethanolamine, piperazine and sodium hydroxide, and the molar ratio of the solution III to the first reaction solution in the step 2 is 2: 1.
the pH value of the first reaction solution in the step 1 is 7.
The pH value of the second reaction solution in the step 2 is 7.
And in the step 4, the ammonium polyphosphate accounts for 30 percent of the finished product in percentage by weight.
According to the test and analysis of the experimental results shown in fig. 2, the carbon residue rate of each of examples 1 to 3 reaches more than 60% at a temperature of 500 ℃, and the carbon residue rate of each of examples 1 to 3 reaches more than 48% at a temperature of 700 ℃, so that the carbon layer has good carbon forming ability, a compact structure, good thermal stability and good flame retardance.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of a phosphorus-containing macromolecular intumescent flame-retardant char-forming agent is characterized by comprising the following steps: the method comprises the following steps:
step 1: pouring cyanuric chloride and ethylenediamine into a bottle, stirring and dissolving to obtain a first solution, stirring the first solution, dropwise adding a second solution into the first solution while stirring, after dropwise adding for more than one hour, injecting nitrogen into the bottle, and reacting the first solution and the second solution for 3 hours under the nitrogen maintenance condition to obtain a first reaction solution, wherein the reaction temperature is 10-15 ℃;
step 2: dropwise adding the solution III into the first reaction solution reacted in the step 1, and stirring the first reaction solution to ensure that the first reaction solution and the solution III are fully reacted to obtain a second reaction solution, wherein the reaction temperature is 50-80 ℃, and the reaction time is 3 hours;
and step 3: dropwise adding the other part of the solution III into the second reaction solution reacted in the step 2, stirring the second reaction solution to enable the second reaction solution and the solution III to fully react, and fully reacting at the reflux temperature for 6-8 hours to obtain a third reaction solution;
and 4, step 4: and (3) cooling the third reaction liquid in the step (3) to room temperature, filtering and washing the third reaction liquid for multiple times by using water and ethanol, adding ammonium polyphosphate into the third reaction liquid, uniformly stirring, and drying in an oven to obtain a finished product, wherein the temperature is 80-110 ℃, and the time is 24 hours.
2. The preparation method of the phosphorus-containing macromolecular intumescent flame retardant char-forming agent according to claim 1, characterized in that: the solution II in the step 1 comprises ethanolamine, alcohol phosphate and triethylamine, and the molar ratio of the solution II to the solution I is 1: 2-5.
3. The preparation method of the phosphorus-containing macromolecular intumescent flame retardant char-forming agent according to claim 1, characterized in that: the solution III in the step 2 comprises ethanolamine, piperazine and sodium hydroxide, and the molar ratio of the solution III to the first reaction solution in the step 2 is 2: 1-2.
4. The preparation method of the phosphorus-containing macromolecular intumescent flame retardant char-forming agent according to claim 1, characterized in that: the pH value of the first reaction solution in the step 1 is 5-7.
5. The preparation method of the phosphorus-containing macromolecular intumescent flame retardant char-forming agent according to claim 1, characterized in that: and the pH value of the second reaction solution in the step 2 is 5-7.
6. The preparation method of the phosphorus-containing macromolecular intumescent flame retardant char-forming agent according to claim 1, characterized in that: and in the step 4, the ammonium polyphosphate accounts for 20-30% of the finished product in percentage by weight.
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| CN113201017A (en) * | 2021-04-29 | 2021-08-03 | 宁波中苑颜料有限公司 | Organic pigment dispersant based on triazine derivative and preparation method thereof |
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| CN113201017B (en) * | 2021-04-29 | 2022-07-01 | 宁波中苑颜料有限公司 | Organic pigment dispersant based on triazine derivative and preparation method thereof |
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