CN109503860B - Modified lignin for intumescent flame retardant and preparation method thereof, intumescent flame retardant and preparation method thereof - Google Patents
Modified lignin for intumescent flame retardant and preparation method thereof, intumescent flame retardant and preparation method thereof Download PDFInfo
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Abstract
The invention relates to modified lignin for an intumescent flame retardant and a preparation method thereof, and the intumescent flame retardant and the preparation method thereof. The raw materials for preparing the modified lignin comprise the following components: alkali lignin, ethylene glycol dimethyl ether, formaldehyde and maleic anhydride; wherein the feeding ratio of the alkali lignin to the glycol dimethyl ether is 1 g: 3 ml-1 g: 5ml of the solution; wherein the mass ratio of the alkali lignin, the formaldehyde and the maleic anhydride is 1: a: b, wherein A is 0.05-0.15, and B is 0.15-0.25. The modified lignin for the intumescent flame retardant prepared from the raw materials contains reactive groups such as hydroxyl, carboxyl and unsaturated double bonds, and can improve the reactivity with other raw materials when being used for the intumescent flame retardant, so that the flame retardant efficiency of the intumescent flame retardant is improved, and the application is facilitated.
Description
Technical Field
The invention relates to the technical field of flame retardants, in particular to modified lignin for an intumescent flame retardant and a preparation method thereof, and the intumescent flame retardant and a preparation method thereof.
Background
The intumescent flame retardant is an environment-friendly green flame retardant, has excellent flame retardant performance, low smoke, low toxicity and no corrosive gas, and is one of the most favored flame retardants at present. The chemical intumescent flame retardant is the most commonly used intumescent flame retardant, and usually a carbon source, a gas source and an acid source are used for synergistic action, so that a carbonaceous foam layer is generated on the surface of the plastic containing the flame retardant during combustion, and the effects of heat insulation, oxygen insulation, smoke suppression and drip prevention are achieved, and the flame retardant effect is achieved. The traditional chemical intumescent flame retardant comprises ammonium polyphosphate (APP), melamine polyphosphate and the like, however, the traditional intumescent flame retardant has low flame retardant efficiency and is not beneficial to application.
Disclosure of Invention
Based on the above, it is necessary to provide a modified lignin for an intumescent flame retardant and a preparation method thereof, and an intumescent flame retardant and a preparation method thereof, aiming at the problem of how to improve the flame retardant efficiency.
The modified lignin for the intumescent flame retardant comprises the following raw materials: alkali lignin, ethylene glycol dimethyl ether, formaldehyde and maleic anhydride;
wherein the feeding ratio of the alkali lignin to the glycol dimethyl ether is 1 g: 3 ml-1 g: 5ml of the solution;
wherein the mass ratio of the alkali lignin, the formaldehyde and the maleic anhydride is 1: a: b, wherein A is 0.05-0.15, and B is 0.15-0.25.
In the raw materials for preparing the modified lignin for the intumescent flame retardant, ethylene glycol dimethyl ether is used as a reaction medium; formaldehyde reacts with alkali lignin, and hydroxyl can be generated on the surface of the alkali lignin; the maleic anhydride reacts with the alkali lignin to generate carboxyl on the surface of the alkali lignin, and simultaneously, the maleic anhydride also has unsaturated double bonds. Therefore, the modified lignin for the intumescent flame retardant prepared by the raw materials contains reactive groups such as hydroxyl, carboxyl and unsaturated double bonds, and when the modified lignin is used for the intumescent flame retardant, the reactivity with other raw materials can be improved, so that the flame retardant efficiency of the intumescent flame retardant is improved, and the application is facilitated.
In one embodiment, the dosage ratio of the alkali lignin to the glycol dimethyl ether is 1 g: 4 ml; the mass ratio of the alkali lignin to the formaldehyde to the maleic anhydride is 1: 0.1: 0.2.
also provides a preparation method of the modified lignin for the intumescent flame retardant, which comprises the following steps:
mixing alkali lignin, ethylene glycol dimethyl ether, formaldehyde and maleic anhydride according to a ratio, maintaining the reaction temperature at 80-90 ℃ and the reaction time at 2-6 h, filtering and retaining filter residue after full reaction, washing the filter residue with water until the pH value is constant, and drying to obtain the modified lignin.
In the preparation method of the modified lignin for the intumescent flame retardant, glycol dimethyl ether is used as a reaction medium; formaldehyde reacts with alkali lignin, and hydroxyl can be generated on the surface of the alkali lignin; the maleic anhydride reacts with the alkali lignin to generate carboxyl on the surface of the alkali lignin, and simultaneously, the maleic anhydride also has unsaturated double bonds. Therefore, the modified lignin for the intumescent flame retardant prepared by the raw materials contains reactive groups such as hydroxyl, carboxyl and unsaturated double bonds, and when the modified lignin is used for the intumescent flame retardant, the reactivity with other raw materials can be improved, so that the flame retardant efficiency of the intumescent flame retardant is improved, and the application is facilitated.
In one embodiment, the reaction temperature is maintained at 80-90 deg.C, and the microwave of 300-500W is used for radiation heating.
The intumescent flame retardant is prepared from the following raw materials in parts by mass:
in the raw materials for preparing the intumescent flame retardant, the modified lignin can improve the reactivity with other raw materials; phosphoric acid and silicic acid can enable the surface of a carrier polymer material to form a firm Si-C foam layer in the combustion process, have better effects of heat insulation, oxygen insulation, smoke suppression and drip prevention, and have a flame retardant effect; the urea can burn to release nitrogen to generate air holes, the air holes are filled with nitrogen, the nitrogen does not support combustion, oxygen can be diluted, and the flame-retardant effect is achieved. The whole can improve the flame-retardant efficiency of the intumescent flame retardant, and is beneficial to application.
In one embodiment, the raw materials for preparing the intumescent flame retardant comprise the following components in parts by mass:
in addition, the preparation method of the intumescent flame retardant is also provided, and comprises the following steps:
according to the mass parts, 1-2 parts of modified lignin, 1-2 parts of phosphoric acid, 1-2 parts of silicic acid and 1-2 parts of urea are fully mixed, the mixture is reacted at the temperature of 90-100 ℃ until bubbles are generated, then the temperature is raised, the reaction temperature is maintained at 190-200 ℃, and the intumescent flame retardant is obtained after full reaction.
In the preparation method of the intumescent flame retardant, the modified lignin can improve the reactivity with other raw materials; phosphoric acid and silicic acid can enable the surface of a carrier polymer material to form a firm Si-C foam layer in the combustion process, have better effects of heat insulation, oxygen insulation, smoke suppression and drip prevention, and have a flame retardant effect; the urea can burn to release nitrogen to generate air holes, the air holes are filled with nitrogen, the nitrogen does not support combustion, oxygen can be diluted, and the flame-retardant effect is achieved. The whole can improve the flame-retardant efficiency of the intumescent flame retardant, and is beneficial to application.
In one embodiment, the reaction is carried out at a temperature of 90 ℃ to 100 ℃, and the microwave of 500W to 1500W is used for radiation heating.
In one embodiment, the reaction temperature is maintained at 190-200 deg.C, and microwave of 2000-3000W is used for radiation heating.
In one embodiment, the time for sufficient reaction is 1.5h to 2.5 h.
Drawings
FIG. 1 is a thermal weight loss (TG) curve of the intumescent flame retardant prepared in examples 1-4.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The modified lignin for the intumescent flame retardant of one embodiment of the invention comprises the following raw materials: alkali lignin, ethylene glycol dimethyl ether, formaldehyde and maleic anhydride.
Wherein the feeding ratio of the alkali lignin to the glycol dimethyl ether is 1 g: 3 ml-1 g: 5 ml.
Wherein the mass ratio of the alkali lignin, the formaldehyde and the maleic anhydride is 1: a: b, wherein A is 0.05-0.15, and B is 0.15-0.25.
Among the above raw materials, alkali lignin is lignin extracted from plant tissues with alkali. Among them, Lignin (Lignin) is an amorphous aromatic high polymer widely existing in plants and having a molecular structure containing structural units of oxyphenbutamol or a derivative thereof. Therefore, the alkali lignin is used as a raw material to prepare the intumescent flame retardant, so that the heat resistance of the product can be improved. In addition, the alkali lignin is derived from papermaking industrial waste, and is used in the intumescent flame retardant, so that the cost of the intumescent flame retardant is greatly reduced.
In the above raw materials, ethylene glycol dimethyl ether is used as a reaction medium to disperse alkali lignin in ethylene glycol dimethyl ether.
In the above raw materials, formaldehyde reacts with alkali lignin to generate hydroxyl groups on the surface of alkali lignin.
In the raw materials, maleic anhydride reacts with alkali lignin to generate carboxyl on the surface of the alkali lignin, and the maleic anhydride also has unsaturated double bonds.
Preferably, the feeding ratio of the alkali lignin to the glycol dimethyl ether is 1 g: 4 ml; the mass ratio of the alkali lignin, the formaldehyde and the maleic anhydride is 1: 0.1: 0.2.
in the raw materials for preparing the modified lignin for the intumescent flame retardant, ethylene glycol dimethyl ether is used as a reaction medium; formaldehyde reacts with alkali lignin, and hydroxyl can be generated on the surface of the alkali lignin; the maleic anhydride reacts with the alkali lignin to generate carboxyl on the surface of the alkali lignin, and simultaneously, the maleic anhydride also has unsaturated double bonds. Therefore, the modified lignin for the intumescent flame retardant prepared by the raw materials contains reactive groups such as hydroxyl, carboxyl and unsaturated double bonds, and when the modified lignin is used for the intumescent flame retardant, the reactivity with other raw materials can be improved, so that the flame retardant efficiency of the intumescent flame retardant is improved, and the application is facilitated.
In addition, the modified lignin contains reactive groups such as hydroxyl, carboxyl, unsaturated double bonds and the like, and can be subjected to surface modification according to the molecular chain structure of the target flame-retardant polymer substrate during polymerization with other raw materials, so that the problem of compatibility between the modified lignin and the substrate is solved, and the modified lignin has good controllability.
The preparation method of the modified lignin for the intumescent flame retardant comprises the following steps:
mixing alkali lignin, ethylene glycol dimethyl ether, formaldehyde and maleic anhydride according to a ratio, maintaining the reaction temperature at 80-90 ℃ and the reaction time at 2-6 h, filtering and retaining filter residue after full reaction, washing the filter residue with water until the pH value is constant, and drying to obtain the modified lignin.
Preferably, the raw materials are added into a reaction kettle with a condensation reflux and tail gas receiving device for reaction. The ethylene glycol dimethyl ether and the formaldehyde are easy to volatilize, so that the volatilized ethylene glycol dimethyl ether and formaldehyde can be refluxed into the reaction kettle again through condensation and reflux, and the loss of raw materials is reduced. Wherein, tail gas receiving arrangement is used for receiving formaldehyde, avoids formaldehyde to arrange to the external world, is favorable to the environmental protection. Specifically, water may be added to the tail gas receiving device, and the characteristic that formaldehyde is soluble in water is utilized to dissolve the discharged formaldehyde in water, so as to receive formaldehyde.
Preferably, the reaction temperature is maintained at 80 ℃ to 90 ℃, and the microwave of 300W to 500W is used for radiation heating. The temperature interval is near the boiling point of the ethylene glycol dimethyl ether, so that the reaction has a high reaction effect at the highest temperature, and excessive gasification of the ethylene glycol dimethyl ether serving as a reaction medium due to overhigh temperature can be avoided. And the mode that adopts microwave heating can carry out even heating to the material in the reation kettle, makes the temperature of the material in the reation kettle even, more is favorable to going on of reaction.
Wherein the pH value is generally 5-6 after being constant.
The reaction process of the preparation method of the modified lignin for the intumescent flame retardant comprises the following steps:
in the preparation method of the modified lignin for the intumescent flame retardant, glycol dimethyl ether is used as a reaction medium; formaldehyde reacts with alkali lignin, and hydroxyl can be generated on the surface of the alkali lignin; the maleic anhydride reacts with the alkali lignin to generate carboxyl on the surface of the alkali lignin, and simultaneously, the maleic anhydride also has unsaturated double bonds. Therefore, the modified lignin for the intumescent flame retardant prepared by the raw materials contains reactive groups such as hydroxyl, carboxyl and unsaturated double bonds, and when the modified lignin is used for the intumescent flame retardant, the reactivity with other raw materials can be improved, so that the flame retardant efficiency of the intumescent flame retardant is improved, and the application is facilitated.
The raw materials for preparing the intumescent flame retardant comprise the following components in parts by mass:
among the raw materials, phosphoric acid and silicic acid can enable the surface of a carrier polymer material to form a firm Si-C foam layer in the combustion process, and the material has better heat insulation, oxygen insulation, smoke suppression and drip prevention effects and has a flame retardant effect.
In the raw materials, the urea can be combusted to release nitrogen to generate air holes, the air holes are filled with the nitrogen, the nitrogen does not support combustion, and the urea can dilute oxygen to play a role in flame retardance. In addition, the cost of the urea is low, and the urea is beneficial to large-scale application.
Preferably, the raw materials for preparing the intumescent flame retardant of one embodiment of the invention comprise the following components in parts by mass:
in the raw materials for preparing the intumescent flame retardant, the modified lignin can improve the reactivity with other raw materials; phosphoric acid and silicic acid can enable the surface of a carrier polymer material to form a firm Si-C foam layer in the combustion process, have better effects of heat insulation, oxygen insulation, smoke suppression and drip prevention, and have a flame retardant effect; the urea can burn to release nitrogen to generate air holes, the air holes are filled with nitrogen, the nitrogen does not support combustion, oxygen can be diluted, and the flame-retardant effect is achieved. The whole can improve the flame-retardant efficiency of the intumescent flame retardant, and is beneficial to application.
The preparation method of the intumescent flame retardant of one embodiment of the invention comprises the following steps:
according to the mass parts, 1-2 parts of modified lignin, 1-2 parts of phosphoric acid, 1-2 parts of silicic acid and 1-2 parts of urea are fully mixed, the mixture is reacted at the temperature of 90-100 ℃ until bubbles are generated, then the temperature is raised, the reaction temperature is maintained at 190-200 ℃, and the intumescent flame retardant is obtained after full reaction.
The raw materials are preferably added into a reactor in proportion for reaction.
Preferably, in the reaction at a temperature of 90 ℃ to 100 ℃, the reaction is carried out by radiant heating using 500W to 1500W of microwave. Not only can ensure the normal reaction, but also can avoid accidents caused by the rapid gas release at high temperature. And the mode of adopting microwave heating can carry out even heating to the material in the reactor, makes the temperature of the material in the reactor even, more is favorable to going on of reaction.
Wherein, in the operation of carrying out the reaction at the temperature of 90-110 ℃ until bubbles are generated, the number of the bubbles is not limited, and the reaction can be carried out until a small amount or a large amount of bubbles are generated.
Preferably, the reaction temperature is maintained at 190-200 deg.C, and microwave of 2000-3000W is used for radiation heating. Not only can ensure the normal operation of the polymerization reaction, but also can avoid the over-high energy consumption. The material in the reactor can be uniformly heated by adopting a microwave heating mode, so that the temperature of the material in the reactor is uniform, and the reaction is more favorably carried out.
Preferably, the time for sufficient reaction is 1.5h to 2.5 h.
In the preparation method of the intumescent flame retardant, the modified lignin can improve the reactivity with other raw materials; phosphoric acid and silicic acid can enable the surface of a carrier polymer material to form a firm Si-C foam layer in the combustion process, have better effects of heat insulation, oxygen insulation, smoke suppression and drip prevention, and have a flame retardant effect; the urea can burn to release nitrogen to generate air holes, the air holes are filled with nitrogen, the nitrogen does not support combustion, oxygen can be diluted, and the flame-retardant effect is achieved. The whole can improve the flame-retardant efficiency of the intumescent flame retardant, and is beneficial to application.
The intumescent flame retardant of the invention is further illustrated below with reference to specific examples.
Example 1
Adding 500g of alkali lignin, 1500ml of ethylene glycol dimethyl ether, 25g of formaldehyde and 75g of maleic anhydride into a reaction kettle with a condensation reflux and tail gas receiving device for mixing, performing radiation heating by adopting 300W of microwave, maintaining the reaction temperature at 80 ℃, reacting for 2 hours, filtering and retaining filter residue after full reaction, washing the filter residue with water until the pH value is constant, and drying to obtain the modified lignin.
Adding 1000g of modified lignin, 1000g of phosphoric acid, 1000g of silicic acid and 1000g of urea into a reactor for mixing, carrying out radiation heating by adopting 500W of microwave, carrying out reaction at the temperature of 90 ℃ until a large amount of bubbles are generated, then carrying out radiation heating by adopting 2000W of microwave, raising the temperature, maintaining the reaction temperature at 190 ℃, and continuing to react for 1.5 hours to obtain the intumescent flame retardant.
Example 2
Adding 500g of alkali lignin, 2000ml of ethylene glycol dimethyl ether, 50g of formaldehyde and 100g of maleic anhydride into a reaction kettle with a condensation reflux and tail gas receiving device for mixing, carrying out radiation heating by adopting 300W of microwave, maintaining the reaction temperature at 85 ℃, reacting for 4 hours, filtering and retaining filter residue after full reaction, washing the filter residue until the pH value is constant, and drying to obtain the modified lignin.
Adding 1000g of modified lignin, 1500g of phosphoric acid, 1500g of silicic acid and 1000g of urea into a reactor for mixing, carrying out radiation heating by adopting 800W of microwave, carrying out reaction at the temperature of 95 ℃ until a large amount of bubbles are generated, then carrying out radiation heating by adopting 2500W of microwave, heating and maintaining the reaction temperature at 195 ℃, and continuing to react for 2 hours to obtain the intumescent flame retardant.
Example 3
Adding 500g of alkali lignin, 2500ml of ethylene glycol dimethyl ether, 75g of formaldehyde and 125g of maleic anhydride into a reaction kettle with a condensation reflux and tail gas receiving device for mixing, performing radiation heating by adopting 500W of microwave, maintaining the reaction temperature at 85 ℃, reacting for 4 hours, filtering and retaining filter residue after full reaction, washing the filter residue with water until the pH value is constant, and drying to obtain the modified lignin.
Adding 1000g of modified lignin, 2000g of phosphoric acid, 2000g of silicic acid and 2000g of urea into a reactor for mixing, carrying out radiation heating by adopting 1500W of microwave, carrying out reaction at the temperature of 100 ℃ until a large amount of bubbles are generated, then carrying out radiation heating by adopting 3000W of microwave, raising the temperature, maintaining the reaction temperature at 200 ℃, and continuing to react for 2.5 hours to obtain the intumescent flame retardant.
Example 4
Adding 500g of alkali lignin, 1500ml of ethylene glycol dimethyl ether, 25g of formaldehyde and 75g of maleic anhydride into a reaction kettle with a condensation reflux and tail gas receiving device for mixing, performing radiation heating by adopting 300W of microwave, maintaining the reaction temperature at 80 ℃, reacting for 2 hours, filtering and retaining filter residue after full reaction, washing the filter residue with water until the pH value is constant, and drying to obtain the modified lignin.
Adding 1000g of modified lignin, 2000g of phosphoric acid, 1000g of silicic acid and 2000g of urea into a reactor for mixing, carrying out radiation heating by adopting 500W of microwave, carrying out reaction at the temperature of 90 ℃ until a large amount of bubbles are generated, then carrying out radiation heating by adopting 2000W of microwave, raising the temperature, maintaining the reaction temperature at 190 ℃, and continuing to react for 1.5 hours to obtain the intumescent flame retardant.
Comparative example 1
Comparative example 1 differs from example 2 in that no formaldehyde is added.
Comparative example 2
Comparative example 2 differs from example 2 in that no maleic anhydride was added.
Comparative example 3
Comparative example 3 differs from example 2 in that no phosphoric acid is added.
Comparative example 4
Comparative example 4 differs from example 2 in that no silicic acid is added.
Comparative example 5
Comparative example 5 differs from example 2 in that no urea is added.
Performance testing
The same mass of the intumescent flame retardants of examples 1-4 were mixed with polylactic acid, and melt extruded and pelletized to obtain polylactic acid materials, and thermal weight loss (TG) analysis was performed to obtain the TG curve of fig. 1. As can be seen from FIG. 1, the polylactic acid materials adopting the intumescent flame retardants of examples 1-4 have more than 70% of carbon residue at 600 ℃, more than 9% of carbon residue at 900 ℃, and higher carbon residue, which indicates that the intumescent flame retardants of examples 1-4 have better flame retardant efficiency.
The same mass of the intumescent flame retardants of examples 1 to 4 and comparative examples 1 to 5 were mixed with polylactic acid, respectively, and subjected to melt extrusion granulation to obtain a polylactic acid material, and subjected to Thermogravimetric (TG) analysis to obtain the residual carbon amount at 600 ℃ as shown in table 1.
TABLE 1 amount of carbon remaining at 600 ℃ for polylactic acid material
| Performance parameter | Residual carbon content at 600 ℃ (%) |
| Example 1 | 71 |
| Example 2 | 72 |
| Example 3 | 73 |
| Example 4 | 75 |
| Comparative example 1 | 55 |
| Comparative example 2 | 50 |
| Comparative example 3 | 49 |
| Comparative example 4 | 47 |
| Comparative example 5 | 52 |
As can be seen from 1, the polylactic acid materials adopting the intumescent flame retardants of examples 1 to 4 have a residual carbon content of more than 70% at 600 ℃, while the polylactic acid materials adopting the intumescent flame retardants of comparative examples 1 to 5 have a residual carbon content of less than 60% at 600 ℃, which indicates that the intumescent flame retardants of examples 1 to 4 have high flame retardant efficiency.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of modified lignin for intumescent flame retardant is characterized by comprising the following steps:
mixing alkali lignin, ethylene glycol dimethyl ether, formaldehyde and maleic anhydride according to a ratio, maintaining the reaction temperature at 80-90 ℃ and the reaction time at 2-6 h, filtering and retaining filter residues after full reaction, washing the filter residues with water until the pH value is constant, and drying to obtain modified lignin;
the alkali lignin has the following structure:
wherein the feeding ratio of the alkali lignin to the glycol dimethyl ether is 1 g: 3 ml-1 g: 5ml of the solution;
wherein the mass ratio of the alkali lignin, the formaldehyde and the maleic anhydride is 1: a: b, wherein A is 0.05-0.15, and B is 0.15-0.25.
2. The process for the preparation of modified lignin for intumescent flame retardants according to claim 1, characterized in that the dosage ratio of said alkali lignin to said glycol dimethyl ether is 1 g: 4 ml; the mass ratio of the alkali lignin to the formaldehyde to the maleic anhydride is 1: 0.1: 0.2.
3. the method for preparing modified lignin for intumescent flame retardants according to claim 1, wherein the constant pH value means a pH value of 5 to 6.
4. The preparation method of the modified lignin for the intumescent flame retardant of claim 1, wherein in the operation of maintaining the reaction temperature at 80-90 ℃, the microwave of 300-500W is adopted for radiation heating.
5. The intumescent flame retardant is characterized in that the raw materials for preparing the intumescent flame retardant comprise the following components in parts by mass:
1-2 parts of modified lignin prepared by the preparation method of any one of claims 1-4;
1-2 parts of phosphoric acid;
1-2 parts of silicic acid; and
1-2 parts of urea.
6. An intumescent flame retardant as claimed in claim 5, characterized in that the raw materials for preparing the intumescent flame retardant comprise, in parts by mass:
1 part of modified lignin;
2 parts of phosphoric acid;
1 part of silicic acid; and
and 2 parts of urea.
7. The preparation method of the intumescent flame retardant is characterized by comprising the following steps:
according to the mass parts, 1-2 parts of modified lignin prepared by the preparation method of any one of claims 1-4, 1-2 parts of phosphoric acid, 1-2 parts of silicic acid and 1-2 parts of urea are fully mixed, the mixture is reacted at the temperature of 90-100 ℃ until bubbles are generated, then the temperature is raised, the reaction temperature is maintained at 190-200 ℃, and the intumescent flame retardant is obtained after full reaction.
8. A process for the preparation of an intumescent flame retardant as claimed in claim 7, wherein the reaction is carried out at a temperature of 90 ℃ to 100 ℃ by radiant heating with 500W to 1500W of microwaves.
9. A process for the preparation of an intumescent flame retardant as claimed in claim 7, wherein the reaction temperature is maintained between 190 ℃ and 200 ℃, and radiant heating is carried out using microwaves of 2000W to 3000W.
10. A process as claimed in claim 7, wherein the time for sufficient reaction is from 1.5 to 2.5 hours.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811522842.8A CN109503860B (en) | 2018-12-13 | 2018-12-13 | Modified lignin for intumescent flame retardant and preparation method thereof, intumescent flame retardant and preparation method thereof |
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| CN201811522842.8A CN109503860B (en) | 2018-12-13 | 2018-12-13 | Modified lignin for intumescent flame retardant and preparation method thereof, intumescent flame retardant and preparation method thereof |
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| CN109503860A CN109503860A (en) | 2019-03-22 |
| CN109503860B true CN109503860B (en) | 2022-04-01 |
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