CN113944067A - Low-smoke halogen-free flame retardant paper and preparation method thereof - Google Patents
Low-smoke halogen-free flame retardant paper and preparation method thereof Download PDFInfo
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- CN113944067A CN113944067A CN202111233249.3A CN202111233249A CN113944067A CN 113944067 A CN113944067 A CN 113944067A CN 202111233249 A CN202111233249 A CN 202111233249A CN 113944067 A CN113944067 A CN 113944067A
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- flame
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- flame retardant
- brucite powder
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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
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
- D21H17/69—Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/12—Coatings without pigments applied as a solution using water as the only solvent, e.g. in the presence of acid or alkaline compounds
-
- 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
- D21H19/00—Coated paper; Coating material
- D21H19/80—Paper comprising more than one coating
- D21H19/84—Paper comprising more than one coating on both sides of the substrate
-
- 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
Abstract
The invention provides low-smoke halogen-free flame retardant paper and a preparation method thereof, belonging to the technical field of flame retardant paper. The brucite powder is used as the main component of the flame retardant for the flame-retardant paper, has good flame-retardant and smoke-suppression effects, can reduce the smoke amount in the combustion process of the paper, can be fully combined with fibers after being organically modified, and can endow the paper with good strength and folding resistance while endowing the paper with the flame-retardant and smoke-suppression effects. According to the invention, the flame-retardant liquid containing the second brucite powder and the antimony trioxide is coated on the surface of the flame-retardant base paper, so that the flame-retardant property of the flame-retardant paper can be further improved. The brucite and the antimony trioxide are used as the flame retardant of the flame retardant paper, so that the use of halogen-containing flame retardant is avoided, toxic and corrosive gases generated at high temperature or during combustion can be reduced, and the paper is more environment-friendly. Meanwhile, the brucite powder is used as the main component of the flame retardant for the flame-retardant paper, has wide sources and low cost, and is suitable for industrial popularization and application.
Description
Technical Field
The invention relates to the technical field of flame retardant paper, in particular to low-smoke halogen-free flame retardant paper and a preparation method thereof.
Background
The flame-retardant paper is a paper base material with special purposes, belongs to the field of special paper, plays a role in the fields of building, insulation, decoration, automobiles, aerospace and the like and cannot be replaced by other materials, and the paper has the characteristics of flame retardance, smoke suppression, high temperature resistance and the like. The research on the flame retardant paper in China is late compared with that in foreign countries, but the paper with excellent performance is obtained. At present, two production methods of the flame retardant paper are mainly used at home, one is to use the fiber with flame retardance as the raw material to make the flame retardant paper; the other method is to prepare the flame retardant paper by coating, adding in slurry, dipping and other methods. The former method is limited in production due to cost and raw material, and for the latter method, the selection of flame retardant is a key factor in producing flame retardant paper.
At present, the existing flame retardants mainly comprise antimony trioxide, decabromodiphenylethane, melamine cyanurate, aluminum hydroxide and the like, have good flame retardant effect, but are not ideal in the aspect of smoke suppression effect. The application of the flame retardant paper in public places is more, and when the casualties are discovered on large-scale fire scenes in most public places, the smoke quantity in the combustion process is too large and the casualties are fumigated to death, so the smoke suppression effect of the flame retardant paper is particularly important.
Disclosure of Invention
In view of the above, the present invention aims to provide a low smoke halogen-free flame retardant paper and a preparation method thereof. The low-smoke halogen-free flame retardant paper provided by the invention has a good smoke suppression effect.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of low-smoke halogen-free flame retardant paper, which comprises the following steps:
(1) mixing the first brucite powder, an organic modifier and water, and sequentially carrying out solid-liquid separation and drying to obtain an organic modified brucite powder;
(2) mixing the pulped fiber pulp with the organic modified brucite powder, and making to obtain flame-retardant base paper;
(3) coating flame-retardant liquid on the surface of the flame-retardant base paper to obtain low-smoke halogen-free flame-retardant paper; the flame-retardant components of the flame-retardant liquid are a second brucite powder and antimony trioxide.
Preferably, the particle size of the first brucite powder is 300-400 meshes; the particle size of the second brucite powder is 6000-8000 meshes.
Preferably, in the step (1), the organic modifier is one or more of starch, sodium dodecyl sulfate, polyethyleneimine, sodium hexametaphosphate and polyaminoamide.
Preferably, the mass ratio of the organic modifier to the first brucite powder is 0.5-1.5: 100.
Preferably, the starch is gelatinized starch, the gelatinization temperature of the gelatinized starch is 90-95 ℃, and the gelatinization time is 20-30 min.
Preferably, the beating degree of the fiber pulp in the step (2) is 40-50 DEG SR, and the beating time is 30-40 min;
the mass concentration of the pulped fiber pulp is 0.6-0.7%.
Preferably, in the step (2), the mass of the organic modified brucite powder is 30-50% of the dry weight of the fiber slurry.
Preferably, the flame retardant liquid comprises the following components in percentage by mass:
preferably, the coating weight of the flame retardant liquid is 35-55 g/m2；
The coating mode is double-sided single-layer coating.
The invention provides the low-smoke halogen-free flame retardant paper prepared by the preparation method, wherein the low-smoke halogen-free flame retardant paper internally contains an organic modified brucite powder, the surface of the low-smoke halogen-free flame retardant paper is coated with a flame retardant liquid, and the flame retardant components of the flame retardant liquid are brucite powder and antimony trioxide.
The invention provides a preparation method of low-smoke halogen-free flame retardant paper, which comprises the following steps: (1) mixing the first brucite powder, an organic modifier and water, and sequentially carrying out solid-liquid separation and drying to obtain an organic modified brucite powder; (2) mixing the pulped fiber pulp with the organic modified brucite powder, and making to obtain flame-retardant base paper; (3) coating flame-retardant liquid on the surface of the flame-retardant base paper to obtain low-smoke halogen-free flame-retardant paper; the flame-retardant components of the flame-retardant liquid are a second brucite powder and antimony trioxide. The brucite powder is used as the main component of the flame retardant for the flame-retardant paper, has good flame-retardant and smoke-suppression effects, can reduce the smoke amount in the combustion process of the paper, can be fully combined with fibers after being organically modified, and can endow the paper with good strength and folding resistance while endowing the paper with the flame-retardant and smoke-suppression effects. According to the invention, the flame-retardant liquid containing the second brucite powder and the antimony trioxide is coated on the surface of the flame-retardant base paper, so that the flame-retardant property of the flame-retardant paper can be further improved. The brucite and the antimony trioxide are used as the flame retardant of the flame retardant paper, and halogen-containing flame retardants are not used, so that toxic and corrosive gases generated at high temperature or during combustion can be reduced, and the paper is more environment-friendly.
Meanwhile, the brucite powder is used as the main component of the flame retardant for the flame-retardant paper, has wide sources and low cost, and is suitable for industrial popularization and application.
Drawings
FIG. 1 is a flow chart of the preparation of the low smoke zero halogen flame retardant paper of the invention.
Detailed Description
The invention provides a preparation method of low-smoke halogen-free flame retardant paper, which comprises the following steps:
(1) mixing the first brucite powder, an organic modifier and water, and sequentially carrying out solid-liquid separation and drying to obtain an organic modified brucite powder;
(2) mixing the pulped fiber pulp with the organic modified brucite powder, and making to obtain flame-retardant base paper;
(3) coating flame-retardant liquid on the surface of the flame-retardant base paper to obtain low-smoke halogen-free flame-retardant paper; the flame-retardant components of the flame-retardant liquid are a second brucite powder and antimony trioxide.
The first brucite powder, the organic modifier and water are mixed, and solid-liquid separation and drying are sequentially carried out to obtain the organic modified brucite powder. In the invention, the particle size of the first brucite powder is preferably 300-400 meshes, and more preferably 350 meshes.
In the present invention, the first brucite powder is preferably obtained by crushing and grinding brucite concentrate. The purity of the brucite concentrate is preferably more than or equal to 85 percent, and more preferably 90-95 percent. The present invention does not require any particular way of crushing and grinding, and can be done using crushing and grinding means well known to those skilled in the art. Before crushing, the brucite concentrate is preferably washed and dried sequentially by the invention to remove impurities from the brucite concentrate.
In the invention, the organic modifier is preferably one or more of starch, sodium dodecyl sulfate, polyethyleneimine, sodium hexametaphosphate and polyaminoamide, and more preferably starch. In the invention, the mass ratio of the organic modifier to the first brucite powder is preferably 0.5-1.5: 100, and more preferably 0.8-1.2: 100. In the invention, in the mixed liquid obtained by mixing the first brucite powder, the organic modifier and water, the mass concentration of the organic modifier is preferably 1-3%, and more preferably 2%.
The invention does not require any particular mixing means, such as stirring, known to the person skilled in the art. In the present invention, the solid-liquid separation method is preferably a method of allowing the mixed solution obtained after mixing to stand for precipitation and pouring out the supernatant liquid. The present invention does not require any special drying means, and may employ drying means known to those skilled in the art.
In the invention, the starch is preferably gelatinized starch, the gelatinization temperature of the gelatinized starch is preferably 90-95 ℃, and the gelatinization time is preferably 20-30 min, and more preferably 25 min.
In the present invention, when the organic modifier is starch, the first portion of brucite powder, the organic modifier and water are preferably mixed in a manner that:
mixing starch with part of water, heating and pasting to obtain pasted starch;
mixing the first brucite powder with the rest water to obtain brucite slurry;
and mixing the gelatinized starch with brucite slurry, and sequentially carrying out solid-liquid separation and drying to obtain the organic modified brucite powder.
According to the invention, the first brucite powder is organically modified, so that the compatibility of the brucite powder and paper fibers can be improved, and the strength of the paper is improved.
After the organic modified brucite powder is obtained, the pulped fiber slurry and the organic modified brucite powder are mixed and copied to obtain the flame-retardant base paper. In the invention, the fiber pulp preferably comprises needle blade pulp and broad-leaved pulp, and the mass ratio of the needle blade pulp to the broad-leaved pulp is preferably 1: 2-4, and more preferably 1: 3.
In the invention, the beating degree of the fiber pulp is preferably 40-50 DEG SR, more preferably 42-46 DEG SR; the pulping time is preferably 30-40 min, and more preferably 35 min; in the invention, the mass concentration of the pulped fiber pulp is preferably 0.6-0.7%.
In the invention, the mass of the organic modified brucite powder is preferably 30-50% of the dry weight of the fiber slurry, and more preferably 35-45%.
The invention does not require any particular mixing means, such as stirring, known to the person skilled in the art. The present invention has no special requirements for the paper making mode, and the paper making mode known to those skilled in the art can be used. After the papermaking, the wet paper after papermaking is preferably dried, and the drying temperature is preferably 90-100 ℃.
After the flame-retardant base paper is obtained, coating flame-retardant liquid on the surface of the flame-retardant base paper to obtain low-smoke halogen-free flame-retardant paper; the flame-retardant components of the flame-retardant liquid are a second brucite powder and antimony trioxide. In the invention, the particle size of the second brucite powder is preferably 6000-8000 meshes, and more preferably 7000 meshes. In the present invention, the source and preparation method of the second brucite powder are the same as those of the first brucite powder, and the difference is only in particle size, which is not described herein again.
In the invention, the mass ratio of the second brucite powder to the antimony trioxide is preferably 7-9: 1, and more preferably 8: 1.
In the invention, the flame retardant liquid preferably comprises the following components in percentage by mass:
the flame retardant liquid comprises 0.7-1.1% of polyvinyl alcohol by mass percentage. In the present invention, the number average molecular weight of the polyvinyl alcohol is preferably 1600 to 1800. In the present invention, the polyvinyl alcohol functions to promote film formation.
The flame retardant liquid comprises 0.5-0.7% of hydroxymethyl cellulose by mass percentage, and more preferably 0.6%. In the present invention, the hydroxymethyl cellulose functions to adjust the viscosity of the flame retardant liquid.
The flame retardant liquid comprises 26-36% by mass of a second brucite powder.
The flame retardant liquid comprises 3-4% of antimony trioxide by mass percentage. In the invention, the second part of brucite powder is compounded with antimony trioxide, so that the flame-retardant requirement can be met, and the dosage of expensive antimony trioxide can be reduced.
The flame retardant liquid comprises the balance of water in percentage by mass.
In the present invention, the preparation method of the flame retardant preferably comprises the following steps:
heating and mixing polyvinyl alcohol, hydroxymethyl cellulose and water to obtain a glue solution;
and mixing a second part of brucite powder, antimony trioxide and the glue solution to obtain the flame-retardant liquid.
In the present invention, the temperature of the heating and mixing is preferably 90 ℃ and the time is preferably 20 min.
In the invention, the coating amount of the flame retardant liquid is preferably 35-55 g/m2More preferably 40 to 50g/m2(ii) a The coating mode is preferably double-sided single-layer coating. The present invention preferably uses a wire plate coater for the coating.
After the coating, the paper is preferably subjected to a dry calendering process in accordance with the invention.
As a specific embodiment of the invention, a preparation flow chart of the low-smoke halogen-free flame retardant paper is shown in FIG. 1.
The invention provides the low-smoke halogen-free flame retardant paper prepared by the preparation method, wherein the low-smoke halogen-free flame retardant paper internally contains an organic modified brucite powder, the surface of the low-smoke halogen-free flame retardant paper is coated with a flame retardant liquid, and the flame retardant liquid comprises the brucite powder and antimony trioxide.
The following examples are provided to illustrate the low smoke zero halogen flame retardant paper and the preparation method thereof, but they should not be construed as limiting the scope of the present invention.
Example 1
Taking a broad-leaved wood pulp board and a needle-leaved wood pulp board according to the mass ratio of 7: 3 pulping with Bulili pulpPulping in a machine, and pulping for 35 minutes to obtain SR paper pulp fiber pulp with the pulping degree of 45 degrees. The fiber slurry is blended into paper pulp fiber slurry with the mass solubility of 0.7 percent, 300ml of paper pulp fiber slurry is taken, the brucite powder modified by starch is added into the pulped paper pulp by 35 percent (accounting for the absolute dry paper pulp) and is stirred uniformly, and the pulp is made on a sheet making machine for standby. Heating 1799 type polyvinyl alcohol 0.2g and 18g water at 90 deg.C, stirring for 20min, adding hydroxymethyl cellulose with mass fraction of 1%, stirring for 5min to obtain glue solution with certain viscosity, weighing 6000 mesh brucite powder 9g and antimony trioxide 1g, mixing, adding into the glue solution, stirring to obtain flame retardant liquid at 35g/m2The coating amount of the paper is coated on the paper sheet by a wire board coater in a double-sided single-layer mode, indexes of relevant paper sheets are detected after drying and calendaring treatment, the tensile index of the paper sheets is measured according to GB/T12914-2008 'determination of tensile strength of paper and paper board', the whiteness index of the paper sheets is measured according to QB/T2804-.
Example 2
Taking a broad-leaved wood pulp board and a needle-leaved wood pulp board according to the mass ratio of 7: and 3, beating in a wary beater for 37 minutes to obtain the SR paper pulp fiber slurry with the beating degree of 47 degrees. The fiber pulp is blended into paper pulp fiber pulp with the mass solubility of 0.7 percent, 300ml of paper pulp fiber pulp is taken, the brucite powder modified by polyethyleneimine is added into the pulped paper pulp by 35 percent (accounting for the absolute dry paper pulp) and is stirred uniformly, and the mixture is processed by sheet making on a sheet making machine for standby. Heating 1799 g polyvinyl alcohol 0.3g and 18g water at 90 deg.C, stirring for 20min, adding hydroxymethyl cellulose 1 wt%, stirring for 5min to obtain a glue solution with certain viscosity, weighing 6000 mesh brucite powder 8g and antimony trioxide 2g, mixing, adding into the glue solution, stirring to obtain flame retardant liquid at 37g/m2The coating amount of the paper is that the paper sheet is coated by a line plate coater on two sides and a single layer, and the paper sheet is inspected after being dried and calenderedThe indexes of the relevant paper are measured, the tensile index of the paper is measured according to GB/T12914-2008 'determination of tensile strength of paper and paperboard', the whiteness index of the paper is measured according to QB/T2804-2006 'determination of whiteness of paper and paperboard', the vertical combustion is detected according to GB/T1465-.
Example 3
Taking a broad-leaved wood pulp board and a needle-leaved wood pulp board according to the mass ratio of 7: and 3, pulping in a Bulboli pulping machine, and pulping for 35 minutes to obtain the SR paper pulp fiber slurry with the pulping degree of 45 degrees. The fiber slurry is blended into paper pulp fiber slurry with the mass solubility of 0.7 percent, 300ml of paper pulp fiber slurry is taken, the brucite powder modified by the sodium hexametaphosphate is added into the pulped paper pulp by the adding amount of 40 percent (accounting for the absolute dry paper pulp), the mixture is stirred uniformly, and the pulp is made for standby on a sheet making machine. Heating 1799 type polyvinyl alcohol 0.2g and 18g water at 90 deg.C, stirring for 20min, adding hydroxymethyl cellulose with mass fraction of 1%, stirring for 5min to obtain glue solution with certain viscosity, weighing 6000 mesh brucite powder 8g and antimony trioxide 2g, mixing, adding into the glue solution, stirring to obtain flame retardant liquid at 40g/m2The coating amount of the paper is coated on the paper sheet by a wire board coater in a double-sided single-layer mode, indexes of relevant paper are detected after drying and calendaring treatment, the tensile strength of the paper sheet is measured according to GB/T12914-2008 'determination of tensile strength of paper and paper board', the whiteness index of the paper sheet is measured according to QB/T2804-2006 'determination of whiteness of paper and paper board', vertical combustion is detected according to GB/T1465-.
Comparative example 1
The difference from example 1 is that the flame retardant liquid was not coated.
Comparative example 2
The difference from example 1 is that no organically modified brucite powder was added.
Comparative example 3
The difference from example 1 is that no flame retardant liquid was applied and no organically modified brucite powder was added.
The results of the performance tests of examples 1-3 and comparative examples 1-3 are shown in Table 1.
TABLE 1 Performance test results of examples 1 to 3 and comparative examples 1 to 3
As can be seen from Table 1, the flame-retardant paper provided by the invention has the advantages of good flame-retardant property, high whiteness, high tensile strength and obvious smoke suppression effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of low-smoke halogen-free flame retardant paper comprises the following steps:
(1) mixing the first brucite powder, an organic modifier and water, and sequentially carrying out solid-liquid separation and drying to obtain an organic modified brucite powder;
(2) mixing the pulped fiber pulp with the organic modified brucite powder, and making to obtain flame-retardant base paper;
(3) coating flame-retardant liquid on the surface of the flame-retardant base paper to obtain low-smoke halogen-free flame-retardant paper; the flame-retardant components of the flame-retardant liquid are a second brucite powder and antimony trioxide.
2. The preparation method according to claim 1, wherein the first brucite powder has a particle size of 300-400 mesh; the particle size of the second brucite powder is 6000-8000 meshes.
3. The preparation method according to claim 1, wherein in the step (1), the organic modifier is one or more of starch, sodium dodecyl sulfate, polyethyleneimine, sodium hexametaphosphate and polyaminoamide.
4. The preparation method according to claim 1 or 3, wherein the mass ratio of the organic modifier to the first brucite powder is 0.5-1.5: 100.
5. The preparation method according to claim 3, wherein the starch is gelatinized starch, the gelatinization temperature of the gelatinized starch is 90 to 95 ℃, and the gelatinization time is 20 to 30 min.
6. The preparation method according to claim 1, characterized in that the beating degree of the fiber pulp in the step (2) is 40-50 ° SR, and the beating time is 30-40 min;
the mass concentration of the pulped fiber pulp is 0.6-0.7%.
7. The preparation method according to claim 1 or 6, wherein in the step (2), the mass of the organically modified brucite powder is 30-50% of the dry weight of the fiber slurry.
8. The preparation method according to claim 1, wherein the flame retardant liquid comprises the following components in percentage by mass:
9. the method according to claim 1 or 8, wherein the amount of the flame retardant is 35 to 55g/m2；
The coating mode is double-sided single-layer coating.
10. The low smoke zero halogen flame retardant paper prepared by the preparation method of any one of claims 1 to 9, wherein the low smoke zero halogen flame retardant paper contains an organic modified brucite powder inside, and the surface of the low smoke zero halogen flame retardant paper is coated with a flame retardant liquid, and the flame retardant components of the flame retardant liquid are brucite powder and antimony trioxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116356605A (en) * | 2023-03-14 | 2023-06-30 | 江西广源化工有限责任公司 | Brucite flame-retardant slurry and preparation method and application thereof |
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2021
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| CN110453538A (en) * | 2019-08-14 | 2019-11-15 | 肥西县创玺建材科技有限公司 | A kind of good PVC wallpaper of wearability |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116356605A (en) * | 2023-03-14 | 2023-06-30 | 江西广源化工有限责任公司 | Brucite flame-retardant slurry and preparation method and application thereof |
| CN116356605B (en) * | 2023-03-14 | 2024-04-02 | 江西广源化工有限责任公司 | Brucite flame-retardant slurry and preparation method and application thereof |
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Application publication date: 20220118 |