CN114427173B - High-flame-retardancy magnesium hydroxide flame-retardant paper and in-situ synthesis method thereof - Google Patents
High-flame-retardancy magnesium hydroxide flame-retardant paper and in-situ synthesis method thereof Download PDFInfo
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- CN114427173B CN114427173B CN202210047397.4A CN202210047397A CN114427173B CN 114427173 B CN114427173 B CN 114427173B CN 202210047397 A CN202210047397 A CN 202210047397A CN 114427173 B CN114427173 B CN 114427173B
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/02—Methods of beating; Beaters of the Hollander type
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F5/00—Dryer section of machines for making continuous webs of paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/34—Ignifugeants
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Abstract
The invention discloses high-flame-retardancy magnesium hydroxide flame-retardant paper and an in-situ synthesis method thereof, and specifically the high-flame-retardancy magnesium hydroxide flame-retardant paper is prepared by adding calcium oxide into a magnesium chloride solution (the molar ratio of the calcium oxide to the magnesium chloride is less than 1), uniformly dispersing, mixing with a cellulose fiber suspension, standing to obtain the cellulose fiber suspension with mixed phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface, making paper by using the cellulose fiber suspension, and drying. According to the invention, the magnesium hydroxide/basic magnesium chloride is synthesized in situ on the surface of the cellulose fiber, so that the loading capacity and the distribution uniformity of the magnesium hydroxide/basic magnesium chloride on the surface of the cellulose fiber are greatly improved, the flame retardant paper is made, the flame retardant property of the flame retardant paper is greatly improved, the synergistic effect of the basic magnesium chloride and the magnesium hydroxide is utilized, the flame retardant efficiency is greatly improved, and the method is suitable for preparing the environment-friendly flame retardant paper with high flame retardant property requirement.
Description
Technical Field
The invention belongs to the technical field of cellulose flame-retardant materials, and particularly relates to high-flame-retardant magnesium hydroxide flame-retardant paper and an in-situ synthesis method thereof.
Background
Paper and paper products are generally made from plant fibers, which are primarily anhydroglucose (C) 6 H 12 O 6 ) The condensate of (2) is a very flammable substance. The flammability of plant fibers determines the flammability of paper and paper products. A great part of real-life fire is caused by paper products, especially the wide application of indoor decoration materials such as wallpaper and the like is aggravatedA fire occurs. With the enhancement of people's fire protection consciousness, the hazard of fire is highly regarded. Therefore, the demand for the flame retardant property of paper is increasing, and the research on the flame retardant paper is also receiving much attention.
Flame retardant paper is generally produced by adding a flame retardant to the inside of paper or coating the surface of paper by processes such as in-pulp addition, impregnation, and coating. The flame retardant can achieve the purpose of flame retardance by one or more ways of blocking the thermal decomposition of fibers, inhibiting the generation of combustible gas or isolating heat from air and diluting the combustible gas. The halogen-free flame retardant can release a large amount of toxic, harmful and corrosive gases such as smoke, hydrogen cyanide, styrene and the like during combustion, and can cause great damage to human beings, so that the halogen-free flame retardant is widely used.
In recent years, halogen-free flame retardants, including red phosphorus, expandable graphite, and intumescent flame retardants, have been used to retard cellulose fiber paper. Red phosphorus has high flame retardant efficiency, but has dark color, and toxic phosphine gas is released in the processing process, so that the application of the red phosphorus in cellulose fiber paper is limited. The expandable graphite has darker color and lower flame-retardant efficiency, and the application of the expandable graphite is limited to a certain extent. In addition, although the intumescent flame retardant has excellent flame retardant performance in the cellulose fiber paper, the intumescent flame retardant is easy to migrate to the surface of the material, which is not favorable for the application of the intumescent flame retardant in the cellulose fiber paper. Inorganic hydroxide such as magnesium hydroxide is the most commonly used green and pollution-free flame retardant at present, has the advantages of flame retardance, smoke suppression, no toxicity, no volatilization and the like, and is widely applied to flame retardant paper. However, as the inorganic hydroxide, magnesium hydroxide particles are liable to aggregate, and there are problems that compatibility with cellulose materials is poor, flame-retardant efficiency is low, high flame-retardant performance cannot be obtained, and the like, to a greater or lesser extent, no matter what means they are added to a sheet.
In conclusion, the development of the magnesium hydroxide flame-retardant paper with high flame-retardant performance is of great significance.
Disclosure of Invention
Aiming at the problems that in the prior art, when the flame retardant paper is prepared by using the magnesium hydroxide flame retardant, the compatibility with cellulose materials is poor, the flame retardant efficiency is low, and paper with high flame retardant property cannot be obtained, the invention provides the magnesium hydroxide flame retardant paper with high flame retardant property and the in-situ synthesis method thereof, and the synergistic effect of the basic magnesium chloride and the magnesium hydroxide greatly improves the flame retardant property of the magnesium hydroxide flame retardant paper.
The invention is realized by the following technical scheme:
an in-situ synthesis method of high-flame-retardant magnesium hydroxide flame-retardant paper comprises the following steps:
(1) Adding calcium oxide into a magnesium chloride solution, and stirring until a uniformly dispersed mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed, wherein the molar ratio of the calcium oxide to the magnesium chloride is less than 1;
(2) Pulping cellulose fiber pulp to form a cellulose fiber suspension, mixing the cellulose fiber suspension with the magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1), and standing to obtain the cellulose fiber suspension with mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) And (3) making the cellulose fiber suspension with the surface deposition and adsorption mixed phase magnesium hydroxide/magnesium chloride/calcium chloride in the step (2) into paper, and drying to obtain the high-flame-retardancy magnesium hydroxide flame-retardant paper.
Further, the magnesium chloride in the step (1) is magnesium chloride hexahydrate or anhydrous magnesium chloride; the cellulose fiber pulp in the step (2) is more than one of softwood pulp, hardwood pulp, cotton pulp and wheat straw pulp.
Further, the mass ratio of the calcium oxide to the magnesium chloride hexahydrate in the step (1) is 1:10 to 50, wherein the mass ratio of the calcium oxide to the anhydrous magnesium chloride is 1 to 2 to 20; the mass ratio of the cellulose fiber pulp to the magnesium chloride hexahydrate in the step (2) is 0.4-5: 1, the mass ratio of the cellulose fiber pulp to the anhydrous magnesium chloride is 1 to 10:1.
further, the mass ratio of the cellulose fiber pulp to the water in the cellulose fiber suspension in the step (2) is 1: and (3) 40-60, wherein the beating degree is 40-90 DEG SR, and the beating treatment of the cellulose fiber is to mechanically treat the cellulose fiber to enable the cellulose fiber to be devillicate.
Further, in the step (2), the mixing time of the cellulose fiber suspension and the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride mixed dispersion liquid is 10 to 30min, and the mixture is kept still for 3 to 72 hours in a sealed manner.
Further, the step (3) of papermaking is to form wet cellulose fiber paper by vacuum filtration of the cellulose fiber suspension on the surface of which the mixed phase of magnesium hydroxide/magnesium chloride/calcium chloride is deposited and adsorbed.
Further, the drying in the step (3) is within a range of 100 to 150 o And C, heating and drying for 10-30min, wherein part of magnesium hydroxide deposited on the surface of the cellulose fiber can continuously react with magnesium chloride under the heating condition to form basic magnesium chloride, and the basic magnesium chloride and unreacted magnesium hydroxide play a synergistic flame-retardant role on the cellulose fiber, so that the flame retardant property of the magnesium hydroxide flame-retardant paper is improved.
In the invention, the high-flame-retardant magnesium hydroxide flame-retardant paper is prepared by the in-situ synthesis method of the high-flame-retardant magnesium hydroxide flame-retardant paper.
In the invention, calcium oxide powder with the molar ratio of less than 1 to magnesium chloride is added into a magnesium chloride solution and fully stirred, wherein calcium oxide reacts with water to form calcium hydroxide, calcium hydroxide continuously reacts with magnesium chloride to form magnesium hydroxide and calcium chloride, part of magnesium hydroxide deposited on the surface of cellulose fibers can continuously react with magnesium chloride under the heating condition in the drying process of paper to form basic magnesium chloride, and the basic magnesium chloride and unreacted magnesium hydroxide play a synergistic flame-retardant role on the cellulose fibers, thereby improving the flame-retardant property of the magnesium hydroxide flame-retardant paper. The cellulose fiber flame-retardant paper loaded with magnesium hydroxide and basic magnesium chloride prepared by the method adopts the in-situ synthesis technology, so that the magnesium hydroxide and the basic magnesium chloride are uniformly distributed on the surface of the cellulose fiber, the aggregation of magnesium hydroxide particles caused by the conventional filling technology is avoided, the adhesion of the magnesium hydroxide and the basic magnesium chloride to the cellulose fiber is strong, and the paper still maintains good uniformity even when the mass ratio of the magnesium chloride hexahydrate to the cellulose fiber is up to 10. In addition, due to the introduction of fibrous alkali type magnesium chloride, the flame retardant property of the paper is greatly improved. Has the advantages of simple process, low cost and suitability for large-scale production.
Advantageous effects
According to the invention, the magnesium hydroxide/basic magnesium chloride is synthesized in situ on the surface of the cellulose fiber, so that the loading capacity and the distribution uniformity of the magnesium hydroxide/basic magnesium chloride on the surface of the cellulose fiber are greatly improved, the flame retardant paper is made, the flame retardant property of the flame retardant paper is greatly improved, the synergistic effect of the basic magnesium chloride and the magnesium hydroxide is utilized, the flame retardant efficiency is greatly improved, and the method is suitable for preparing the environment-friendly flame retardant paper with high flame retardant property requirement.
Drawings
FIG. 1 is an SEM image of an in-situ deposited magnesium hydroxide/magnesium oxychloride flame retardant paper (example 1) prepared in example 1
FIG. 2 is a photograph of a highly filled flame retardant paper containing magnesium hydroxide/magnesium oxychloride (example 1).
Detailed Description
The present invention is further described with reference to the following specific examples, which are implemented on the premise of the technical solution of the present invention, and give detailed implementation manners and specific operation processes, but the scope of the present invention is not limited to the following examples; unless otherwise indicated, the parts described in the examples are parts by mass.
Example 1
(1) Dispersing 5 parts of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion is formed;
(2) Dispersing 2 parts of softwood pulp into 100 parts of deionized water, fluffing, pulping to 90-degree SR to obtain a cellulose fiber suspension, mixing with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) under stirring for 30 minutes, sealing, and standing for 72 hours to ensure that the magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of the cellulose fiber to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase magnesium hydroxide/magnesium chloride/calcium chloride surface deposited and absorbed in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 150 DEG o Drying for 10 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 220s.
Example 2
(1) Dispersing 4 parts of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion is formed;
(2) Dispersing 4 parts of softwood pulp into 240 parts of deionized water, beating to 80-degree SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) for 20 minutes under stirring, sealing, and standing for 24 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension subjected to surface deposition and adsorption of mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 130 DEG C o Drying for 15 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardant-performance magnesium hydroxide flame-retardant paper is cut into paper strips of 1cm multiplied by 2cm, and the paper strips are directly ignited by an alcohol burner and timed, wherein the burning time is 189s.
Example 3
(1) Dispersing 3 parts of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion is formed;
(2) Dispersing 6 parts of hardwood pulp into 300 parts of deionized water, beating to 60-degree SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) for 15 minutes under stirring, sealing, and standing for 3 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase of magnesium hydroxide/magnesium chloride/calcium chloride deposited and absorbed on the surface in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet on a paper feeding device 100 o Drying for 30 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 171s.
Example 4
(1) Dispersing 1 part of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 5 parts of hardwood pulp into 200 parts of deionized water, beating to 50-DEG SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) under stirring for 15 minutes, sealing, and standing for 8 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension subjected to surface deposition and adsorption of mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 120 DEG C o Drying for 20 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 153s.
Example 5
(1) Dispersing 2 parts of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 6 parts of linter pulp into 300 parts of deionized water, defibering, pulping to 70-DEG SR to obtain a cellulose fiber suspension, mixing with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) under stirring for 10 minutes, sealing, and standing for 12 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension subjected to surface deposition and adsorption of mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet on a paper feeding device 100 o Drying for 30 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardant magnesium hydroxide flame-retardant paper;
cutting the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper into 1cm multiplied by 2cm paper strips, directly igniting and timing by using an alcohol burner, and keeping the burning time at 181s.
Example 6
(1) Dispersing 1 part of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 4 parts of wheat straw pulp into 100 parts of deionized water, beating to 40 DEG SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) for 15 minutes under stirring, sealing, and standing for 48 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase of magnesium hydroxide/magnesium chloride/calcium chloride deposited and absorbed on the surface in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet on a paper feeding device 100 o Drying for 30 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 154s.
Example 7
(1) Dispersing 2 parts of anhydrous magnesium chloride in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 2 parts of softwood pulp into 100 parts of deionized water, fluffing, pulping to 85 DEG SR to obtain a cellulose fiber suspension, mixing with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) under stirring for 30 minutes, sealing, and standing for 60 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of the cellulose fiber to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase magnesium hydroxide/magnesium chloride/calcium chloride surface deposited and absorbed in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 150 DEG o Drying for 10 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 218s.
Example 8
(1) Dispersing 1 part of anhydrous magnesium chloride in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 3 parts of hardwood pulp into 150 parts of deionized water, beating to 60-degree SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) for 30 minutes under stirring, sealing, and standing for 48 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase magnesium hydroxide/magnesium chloride/calcium chloride surface deposited and absorbed in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 130 DEG o Drying for 15 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 192s.
Example 9
(1) Dispersing 0.4 part of anhydrous magnesium chloride in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 2 parts of linter pulp into 100 parts of deionized water, defibering, pulping to 70-DEG SR to obtain a cellulose fiber suspension, mixing with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) under stirring for 20 minutes, sealing, and standing for 24 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase magnesium hydroxide/magnesium chloride/calcium chloride surface deposited and absorbed in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 120 DEG o Drying for 20 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 186s.
Example 10
(1) Dispersing 0.2 part of anhydrous magnesium chloride in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 2 parts of wheat straw pulp into 100 parts of deionized water, beating to 50 DEG SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) for 20 minutes under stirring, sealing, and standing for 12 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase of magnesium hydroxide/magnesium chloride/calcium chloride deposited and absorbed on the surface in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet on a paper feeding device 100 o Drying for 30 minutes to promote partial magnesium hydroxide to react with magnesium chloride to form basic magnesium chloride, thereby obtaining the high-flame-retardancy magnesium hydroxide flame-retardant paper;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into 1cm multiplied by 2cm paper strips, and the paper strips are directly ignited by an alcohol burner and timed, and the burning time is 177s.
Comparative example 1
(1) Dispersing 8 parts of magnesium chloride hexahydrate in 10 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.2 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/calcium chloride dispersion liquid is formed;
(2) Dispersing 2 parts of softwood pulp into 100 parts of deionized water, beating to 90-degree SR after defibering to obtain a cellulose fiber suspension, mixing the cellulose fiber suspension with the mixed-phase magnesium hydroxide/calcium chloride dispersion liquid in the step (1) for 30 minutes under stirring, sealing, and standing for 72 hours to ensure that the mixed-phase magnesium hydroxide/calcium chloride is fully adsorbed on the surface of cellulose fibers to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension subjected to surface deposition and adsorption of mixed-phase magnesium hydroxide/calcium chloride in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 150 DEG C o Drying for 10 minutes under C to obtain the magnesium hydroxide flame-retardant paper with high flame-retardant property;
the prepared high-flame-retardancy magnesium hydroxide flame-retardant paper is cut into 1cm multiplied by 2cm paper strips, and the paper strips are directly ignited by an alcohol burner and timed, and the burning time is 137s.
Comparative example 2
(1) Dispersing 0.2 part of anhydrous magnesium chloride in 15 parts of deionized water, stirring until the magnesium chloride is completely dissolved to obtain a magnesium chloride aqueous solution, and then dispersing 0.1 part of calcium oxide powder in the magnesium chloride aqueous solution under stirring until a uniform mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid is formed;
(2) Dispersing 2 parts of softwood pulp into 100 parts of deionized water, fluffing, pulping to 90-degree SR to obtain a cellulose fiber suspension, mixing with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1) under stirring for 30 minutes, sealing, and standing for 72 hours to ensure that the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride is fully adsorbed on the surface of the cellulose fiber to obtain the cellulose fiber suspension with the mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Forming the cellulose fiber suspension with the mixed phase magnesium hydroxide/magnesium chloride/calcium chloride surface deposited and absorbed in the step (2) through vacuum filtration to obtain a wet paper sheet, and placing the wet paper sheet at 150 DEG o Drying for 10 minutes under C, and reacting magnesium hydroxide with magnesium chloride to form basic magnesium chloride to obtain basic magnesium chloride flame-retardant paper with high flame retardance;
the prepared basic magnesium chloride flame-retardant paper is cut into strips of 1cm multiplied by 2cm, and the strips are directly ignited by an alcohol burner and timed, wherein the burning time is 128s.
Claims (6)
1. An in-situ synthesis method of high-flame-retardancy magnesium hydroxide flame-retardant paper is characterized by comprising the following steps:
(1) Adding calcium oxide powder into a magnesium chloride solution, and stirring to form a uniformly dispersed mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid, wherein the molar ratio of calcium oxide to magnesium chloride is less than 1;
(2) Pulping cellulose fiber pulp to form a cellulose fiber suspension, mixing the cellulose fiber suspension with the magnesium hydroxide/magnesium chloride/calcium chloride dispersion liquid in the step (1), and standing to obtain the cellulose fiber suspension with mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride deposited and adsorbed on the surface;
(3) Making paper from the cellulose fiber suspension with surface deposition and adsorption mixed phase magnesium hydroxide/magnesium chloride/calcium chloride in the step (2), and drying to obtain the magnesium hydroxide flame retardant paper with high flame retardance;
mixing the cellulose fiber suspension in the step (2) with a mixed-phase magnesium hydroxide/magnesium chloride/calcium chloride mixed dispersion liquid for 10 to 30min, and standing for 3 to 72 hours in a sealed manner;
the drying in the step (3) is within a range of 100 to 150 o And C, heating and drying for 10 to 30min.
2. The in situ synthesis method according to claim 1, wherein the magnesium chloride in step (1) is magnesium chloride hexahydrate or anhydrous magnesium chloride; the cellulose fiber pulp in the step (2) is more than one of softwood pulp, hardwood pulp, cotton pulp and wheat straw pulp.
3. The in-situ synthesis method according to claim 2, wherein the mass ratio of the calcium oxide to the magnesium chloride hexahydrate in the step (1) is 1:10 to 50, wherein the mass ratio of the calcium oxide to the anhydrous magnesium chloride is 1 to 2 to 20; the mass ratio of the cellulose fiber pulp to the magnesium chloride hexahydrate in the step (2) is 0.4-5: 1, the mass ratio of the cellulose fiber pulp to the anhydrous magnesium chloride is 1 to 10:1.
4. the in situ synthesis method according to claim 1, wherein the mass ratio of the cellulose fiber pulp to the water in the cellulose fiber suspension in step (2) is 1:40 to 60 degrees, and the beating degree is 40 to 90 degrees SR.
5. The in-situ synthesis method according to claim 1, wherein the step of papermaking in step (3) is to form a wet cellulose fiber paper by vacuum filtration of the cellulose fiber suspension on which the mixed phase of magnesium hydroxide/magnesium chloride/calcium chloride is deposited and adsorbed.
6. The high flame retardant magnesium hydroxide flame retardant paper prepared by the in-situ synthesis method of the high flame retardant magnesium hydroxide flame retardant paper according to any one of claims 1 to 5.
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