CN116874701A - Preparation method of reactive melamine resin - Google Patents
Preparation method of reactive melamine resin Download PDFInfo
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- CN116874701A CN116874701A CN202211164121.0A CN202211164121A CN116874701A CN 116874701 A CN116874701 A CN 116874701A CN 202211164121 A CN202211164121 A CN 202211164121A CN 116874701 A CN116874701 A CN 116874701A
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- melamine resin
- reactive
- reactive melamine
- reduced pressure
- melamine
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 42
- 239000004640 Melamine resin Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 12
- LXCYSACZTOKNNS-UHFFFAOYSA-N diethoxy(oxo)phosphanium Chemical compound CCO[P+](=O)OCC LXCYSACZTOKNNS-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 9
- 229930040373 Paraformaldehyde Natural products 0.000 claims abstract description 6
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 6
- 230000001105 regulatory effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 4
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229920005862 polyol Polymers 0.000 claims description 8
- 150000003077 polyols Chemical class 0.000 claims description 8
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 239000003002 pH adjusting agent Substances 0.000 claims description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- 150000001412 amines Chemical class 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000003384 small molecules Chemical class 0.000 claims description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000035484 reaction time Effects 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
- 239000003063 flame retardant Substances 0.000 description 20
- 230000002195 synergetic effect Effects 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000004814 polyurethane Substances 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 5
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 5
- 229920000570 polyether Polymers 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 5
- BNCADMBVWNPPIZ-UHFFFAOYSA-N 2-n,2-n,4-n,4-n,6-n,6-n-hexakis(methoxymethyl)-1,3,5-triazine-2,4,6-triamine Chemical compound COCN(COC)C1=NC(N(COC)COC)=NC(N(COC)COC)=N1 BNCADMBVWNPPIZ-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 239000004114 Ammonium polyphosphate Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 description 2
- -1 dimethyl (ethyl) methylphosphonate Chemical compound 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical class OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 125000001033 ether group Chemical group 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical class O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- YACKEPLHDIMKIO-UHFFFAOYSA-N methylphosphonic acid Chemical compound CP(O)(O)=O YACKEPLHDIMKIO-UHFFFAOYSA-N 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
Classifications
-
- 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
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method of reactive melamine resin, which comprises the following steps of adding melamine, paraformaldehyde, methanol and polyalcohol into a reaction kettle according to a molar ratio of 1:4-6:2-4:2-4 to form a material I; heating under stirring, and when the temperature of the materials in the reaction kettle is 50-75 ℃, regulating the pH of the system to 9-11 and the reaction time to 2-3 h to obtain a material II; diethyl phosphite is added in a dropwise manner under normal pressure for 10-60 min, wherein the diethyl phosphite is 1-3.5 times of the mole number of melamine, and a material III is obtained; reacting the material III at 50-75 ℃ for 2-4 hours, and then adjusting the pH value to 7-8 to obtain a material IV; and (3) carrying out reduced pressure distillation on the material IV to separate out micromolecule substances in the system, wherein the reduced pressure distillation temperature is 70-100 ℃, the pressure is-0.08 to-0.10 MPa, and the moisture test is less than 0.5% by a gauge pressure meter to obtain the reactive melamine resin.
Description
Technical Field
The invention relates to a preparation method of reactive melamine resin.
Background
Polyurethane rigid foam (PUR) is a heat insulating material and a structural material with excellent performance, has strong adhesion to a base material, and is widely applied to the fields of external walls, pipelines, refrigerator heat preservation and the like. However, the PUR structure is loose and porous and easy to burn, and the flame retardant property of the PUR structure becomes one of key technologies which can be widely used in the future. The method for improving the flame retardant property of the material mainly uses a flame retardant. Common additive flame retardants include halogenated phosphates, non-halogenated phosphonates such as dimethyl (ethyl) methylphosphonate, inorganic flame retardants such as ammonium polyphosphate (APP), encapsulated red phosphorus, expanded graphite, and the like. The added flame retardant may cause problems such as low compatibility, precipitation, and mechanical property degradation. The reactive flame retardant forms a covalent bond with polyurethane, has the advantages of good compatibility, good flame retardant effect under the condition of keeping the inherent mechanical property and low concentration of the polyurethane, and the like, and is paid attention to.
Melamine is the most commonly used nitrogen flame retardant, melamine resin is also called melamine resin, and has a certain flame retardant property because of containing N element in the structure, but the flame retardant effect of single N element is not ideal, so that P element is introduced into melamine resin, and the flame retardant synergistic effect can be formed between the N, P flame retardant elements, so that the flame retardant effect can be enhanced.
Chinese patent CN110283207a discloses a phosphorus-nitrogen synergic flame retardant polyether polyol resin, which has the following structural formula: wherein r=r 1 Or n is more than or equal to 2 and less than or equal to 4, m is more than or equal to 2 and less than or equal to 4, and x is more than or equal to 1. A preparation method of phosphorus-nitrogen synergistic flame-retardant polyether polyol resin comprises the following steps: and heating hexamethoxymethyl melamine (HMMM) and phosphate dihydric alcohol or aliphatic dihydric alcohol under the catalysis of p-toluenesulfonic acid to carry out an ether exchange reaction, and carrying out post-treatment to obtain the phosphorus-nitrogen synergistic polyether polyol resin with polyhydroxy. The process has complex reaction conditions and high cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a novel preparation method of reactive melamine resin, and the prepared reactive melamine resin has the advantages of good flame retardant property, lasting flame retardant property, no toxicity and small influence on environment.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the reactive melamine resin sequentially comprises the following steps:
(1) Adding melamine, paraformaldehyde, methanol and polyalcohol into a reaction kettle according to a molar ratio of 1:4-6:2-4:2-4 to form a material I;
(2) Heating under stirring, adding a pH regulator when the temperature of the materials in the reaction kettle is 50-75 ℃, regulating the pH of the system to 9-11, and reacting for 2-3 h to obtain a material II;
(3) Diethyl phosphite is added in a dropwise manner under normal pressure, wherein the dropwise time is 10-60 min, and the mass of the diethyl phosphite is 1-3.5 times of the mole number of melamine, so that a material III is obtained;
(4) Reacting the material III at 50-75 ℃ for 2-4 h, then adding a pH regulator, and regulating the pH to 7-8 to obtain a material IV;
(5) And (3) carrying out reduced pressure distillation on the material IV to separate out micromolecule substances in the system, wherein the reduced pressure distillation temperature is 70-100 ℃, the pressure is-0.08 to-0.10 MPa, and the moisture test is less than 0.5% by a gauge pressure meter to obtain the reactive melamine resin.
In the above technical solution, preferably, the polyol in the step (1) is at least one selected from ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, butylene glycol and glycerin.
In the above technical solution, preferably, the pH adjusting agent in the step (2) is at least one of aqueous solution of sodium hydroxide, potassium hydroxide or organic amine with basicity; the pH is adjusted to 9-11.
In the above technical solution, preferably, the pH adjusting agent in the step (4) is at least one of aqueous solution of sodium hydroxide, potassium hydroxide or organic amine with basicity; the pH is regulated to 7-8.
In the above technical solution, preferably, the small molecule byproduct in the step (5) is a mixture of free formaldehyde, water and methanol.
In the above technical scheme, preferably, the reduced pressure distillation temperature in the step (5) is 70-100 ℃.
In the above technical scheme, preferably, the structural feature of the reactive melamine resin prepared in the step (5) is as follows:
wherein: r is-O (C) 2 H 4 O) m H、-O(CH 2 CH(CH 3 )O) n H、-OCH 2 CH(OH)CH 2 OH or-
O(CH 2 ) 4 One of OH; wherein m is more than or equal to 1 and less than or equal to 2, n is more than or equal to 1 and less than or equal to 2;
r1=r orWherein the general formula (I) is a main product.
The invention provides a preparation method of reactive melamine resin, which is characterized in that flame retardant element phosphorus is introduced into a melamine molecular structure to achieve a synergistic flame retardant effect of phosphorus and nitrogen, and the structure contains more than two reactive groups-OH, specifically, melamine, paraformaldehyde, methanol and polyol are added into a reaction container according to a certain molar ratio, the melamine and the paraformaldehyde undergo methylolation reaction under the catalysis of alkali to generate methylol melamine, diethyl phosphite and the methylol melamine react to generate melamine phosphate diol, and the methylol melamine and the methanol undergo etherification reaction under the catalysis of the acid condition of diethyl phosphite to generate methylated melamine formaldehyde resin, and the methylated melamine resin and the polyol react to generate melamine resin with a certain functionality to finally obtain the reactive melamine resin, so that a better technical effect is achieved.
Detailed Description
The following is a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, but rather the technical solutions falling under the concept of the present invention should fall within the scope of the present invention, and for those skilled in the art, the minor modifications and the modifications made to the present invention without departing from the principles of the present invention should fall within the scope of the present invention.
[ example 1 ]
(1) Adding melamine, paraformaldehyde, methanol and diglycol into a reaction vessel according to a molar ratio of 1:4:2:2, and uniformly stirring to obtain a material I;
(2) Heating the material I to 50 ℃, adding triethylamine, adjusting the pH to be 9, and reacting at normal pressure for 2 hours to obtain a material II;
(3) Dropwise adding diethyl phosphite into the material II for 30min, wherein the molar ratio of the added diethyl phosphite to the melamine in the step (1) is 2:1, obtaining a material III;
(4) Keeping the temperature of the material III at 50 ℃, continuing to react for 2 hours, adding triethylamine, and adjusting the pH value to be 7.5 to obtain a material IV;
(5) Distilling the material IV under reduced pressure to remove small molecule byproducts, filtering to remove solid salt by using a gauge pressure meter at the reduced pressure distillation temperature of 75 ℃ and the pressure of-0.098 MPa to obtain the reactive melamine resin S 1 The performance data are shown in Table 2.
Examples 2 to 6
Examples 2 to 6 were carried out according to the steps of example 1, except that the reaction raw materials, the raw material ratios, the types and the amounts of the catalysts, the reaction time, the reaction temperature, the pH adjusting agent and the adjusted pH value were all obtained, wherein the concentrations of the pH adjusting agent were mass percent concentrations, and the reaction conditions were specifically shown in Table 1.
Table 1 examples 1 to 6 raw material molar ratio and reaction conditions in the preparation of reactive melamine resin
[ comparative example 1 ]
1. Referring to the procedure in example 1 of patent CN110283207A, a phosphorus-nitrogen synergistic flame retardant polyether polyol was synthesized as follows:
hexamethoxymethyl melamine (HMMM, 3.9g,0.01 mol) and a phosphate glycol (diethyl bis-2-hydroxyethyl amine methylphosphonate, FRC-6,5.1g,0.02 mol) were added to a 100mL three-necked flask, p-toluenesulfonic acid (TsOH, about 0.005 g) and N, N-dimethylformamide (DMF, 2 g) were added thereto, and the mixture was magnetically stirred at 120℃under nitrogen for 3 hours to complete the transesterification reaction; cooling the reaction system to room temperature, adding 2mL of ethyl acetate, stirring uniformly, then adding 12mL of n-hexane under stirring, standing for phase separation, and removing supernatant; repeating the steps for 3 to 5 times, and rotationally evaporating the sticky substance at the lower layer at the temperature of 55 to 70 ℃ to remove the solvent to obtain a brown yellow sticky product: the yield of the phosphorus-nitrogen synergic flame-retardant polyether glycol is 95%.
TABLE 2 index data for reactive melamine resins prepared in examples 1 to 6 and comparative example 1
As can be seen from the performance data in Table 2, the conventional index performance data of the reactive melamine resins prepared in examples 1 to 6 of the present application are similar to those of comparative example 1, and the preparation process is simple, the cost is low, the process adjustment scheme of the present invention is adopted, the operation is simple, the cost of the prepared reactive melamine resin can be reduced on the premise of not influencing the conventional performance index, and a good technical effect is obtained, so that the reactive melamine resin can be used in polyurethane foam application.
Claims (5)
1. The preparation method of the reactive melamine resin sequentially comprises the following steps:
(1) Adding melamine, paraformaldehyde, methanol and polyalcohol into a reaction kettle according to a molar ratio of 1:4-6:2-4:2-4 to form a material I;
(2) Heating under stirring, adding a pH regulator when the temperature of the materials in the reaction kettle is 50-75 ℃, regulating the pH of the system to 9-11, and reacting for 2-3 h to obtain a material II;
(3) Diethyl phosphite is added in a dropwise manner under normal pressure, wherein the dropwise time is 10-60 min, and the mass of the diethyl phosphite is 1-3.5 times of the mole number of melamine, so that a material III is obtained;
(4) Reacting the material III at 50-75 ℃ for 2-4 h, then adding a pH regulator, and regulating the pH to 7-8 to obtain a material IV;
(5) And (3) carrying out reduced pressure distillation on the material IV to separate out micromolecule substances in the system, wherein the reduced pressure distillation temperature is 70-100 ℃, the pressure is-0.08 to-0.10 MPa, and the moisture test is less than 0.5% by a gauge pressure meter to obtain the reactive melamine resin.
2. The method for preparing reactive melamine resin according to claim 1, wherein the polyol in the step (1) is at least one selected from the group consisting of ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, butylene glycol and glycerin.
3. The method for producing a reactive melamine resin according to claim 1, wherein the pH adjusting agent in the step (2) and the step (4) is at least one of an aqueous solution of sodium hydroxide, potassium hydroxide or an organic amine that is basic.
4. The method for preparing reactive melamine resin according to claim 1, wherein the small molecule by-product in the step (5) is a mixture of free formaldehyde, water and methanol.
5. The process for producing a reactive melamine resin according to claim 1, where in the reduced pressure distillation temperature in step (5) is 75 to 95 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211164121.0A CN116874701A (en) | 2022-09-23 | 2022-09-23 | Preparation method of reactive melamine resin |
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| CN202211164121.0A CN116874701A (en) | 2022-09-23 | 2022-09-23 | Preparation method of reactive melamine resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117384425A (en) * | 2023-12-12 | 2024-01-12 | 山东理工大学 | Polyurethane hard bubble oxygen index chemical regulator and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117384425A (en) * | 2023-12-12 | 2024-01-12 | 山东理工大学 | Polyurethane hard bubble oxygen index chemical regulator and preparation method and application thereof |
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