CN115216993A - Method for preparing hydrophobic flame-retardant paper by coating - Google Patents
Method for preparing hydrophobic flame-retardant paper by coating Download PDFInfo
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- CN115216993A CN115216993A CN202210597051.1A CN202210597051A CN115216993A CN 115216993 A CN115216993 A CN 115216993A CN 202210597051 A CN202210597051 A CN 202210597051A CN 115216993 A CN115216993 A CN 115216993A
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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
- D21H21/16—Sizing or water-repelling agents
-
- 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
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/07—Nitrogen-containing 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
-
- 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
- D21H17/64—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
- D21H19/10—Coatings without pigments
-
- 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
-
- 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
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
- D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
Abstract
The invention relates to a method for preparing hydrophobic flame-retardant paper by coating, which comprises the steps of preparing a hydrophobic modified flame retardant by a sol-gel method; preparing a hydrophobic flame-retardant coating; the hydrophobic flame-retardant paper is prepared by a coating method. By adopting the invention, the paper has the hydrophobic flame retardant characteristic, the flame retardant is converted from hydrophilicity to hydrophobicity, the flame retardant can not be separated out by moisture absorption on the surface of the paper, and the Cobb value is26.1g/m 2 The LOI is 30.2%, and the flame retardant has the characteristics of good hydrophobic flame retardant property, simple equipment, easiness in industrial batch production and the like.
Description
Technical Field
The invention belongs to a preparation method of hydrophobic flame-retardant paper, and belongs to the field of special paper manufacturing.
Background
The paper used as wood fiber reshaping material has the advantages of low cost, light weight, easy processing, high strength, excellent printing adaptability, convenient storage and transportation and the like, and is widely applied to the fields of packaging materials, building materials and the like.
The paper is a three-dimensional porous net-shaped structure material formed by interweaving countless long-chain cellulose molecules. Cellulose (C) 6 H 10 O 5 ) n The glucose-based polymer is a linear high polymer formed by connecting D-glucopyranose through beta- (1 → 4) glycosidic bonds, each glucose unit contains 3 active hydroxyl groups (-OH), and intermolecular and intramolecular hydrogen bonds can be formed among the hydroxyl groups. Because a large number of hydrogen bonds easy to hydrolyze exist among basic units of the cellulose and a three-dimensional porous network structure of the paper, the paper has natural strong hydrophilicity, water molecules easily permeate into paper fibers and diffuse to damage the fiber networkThe hydrogen bonds in the network are combined, so that the integral structure of the paper is damaged, and the mechanical strength and the mechanics are reduced.
Meanwhile, the structure of the paper also determines the characteristic of extremely easy combustion of the paper, so that the production of the plant fiber flame retardant paper needs to add flame retardant materials by different methods to obtain a better flame retardant effect, however, most flame retardants have hydrophilicity, the problems of flame retardant loss, deteriorated flame retardant performance and the like can occur in a humid environment, the paper with hydrophilicity is also extremely easy to be polluted by stains, the moisture absorption of the flame retardants can enable the surface of the paper to become humid and be not beneficial to storage, and various performance indexes of the paper are also affected, so that the application of the paper in some special fields is limited due to the hydrophilicity and the inflammability of the paper. If we can add waterproofing agent and fire retardant by coating way to get the paper with hydrophobic fire retardant property, it can expand its application scope and increase its durability.
Disclosure of Invention
The invention aims to provide a method for preparing hydrophobic modified flame retardant by a sol-gel method, which ensures that the flame retardant does not generate moisture absorption and precipitation on the surface of paper after coating, thereby improving the physical properties and the flame retardant effect of the paper and ensuring that the paper has good hydrophobic flame retardant property.
The technical scheme adopted by the invention is as follows: a method for preparing hydrophobic flame-retardant paper by coating is characterized by comprising the following steps:
(1) Preparing a hydrophobic modified flame retardant by a sol-gel method; pouring ethanol and deionized water in a certain proportion into a three-neck flask at the temperature of 30-50 ℃, and uniformly stirring by using a stirrer to obtain an ethanol solution; adding 50g of fire retardant into 200g of ethanol solution, and uniformly stirring; sequentially adding a surfactant OP-10 and ammonia water, and uniformly stirring; slowly and dropwise adding ethyl orthosilicate into a reaction system, uniformly stirring and fully reacting; then, dropwise adding a silane coupling agent to react for 3-5 hours; finally, cooling the product to room temperature, filtering, washing with water and absolute ethyl alcohol respectively twice, and drying at 80 ℃ to obtain the hydrophobic modified flame retardant;
(2) Preparing a hydrophobic flame-retardant coating; mixing the hydrophobic modified flame retardant and the styrene-acrylic emulsion in a certain proportion, wherein the addition amount of the hydrophobic modified flame retardant accounts for 50-65% of the total mass of the hydrophobic flame-retardant coating;
(3) Preparing hydrophobic flame-retardant paper by a coating method; coating the base paper with the coating amount of the hydrophobic flame-retardant coating being 8-16% of the mass of the base paper, drying the coated paper at 105 ℃ for 30 minutes, heating to 160 ℃ for curing for 10 minutes, and cooling to room temperature to obtain the hydrophobic flame-retardant paper.
Further, the volume ratio of the absolute ethyl alcohol to the deionized water in the step (1) is 1-2: 1, and the volume ratio of the ammonia water to the whole solvent system is 6-9: 100; the mass ratio of the tetraethoxysilane to the flame retardant is 0.6-1: 5.
Further, the flame retardant in the step (1) is melamine cyanurate and aluminum hydroxide, and the mass ratio is 4-6: 6-4.
Further, in the step (1), the silane coupling agent is one or two of n-octyl triethoxysilane, ethyl triethoxysilane and gamma-methacryloxypropyl trimethoxysilane, and the mass ratio of the silane coupling agent to the flame retardant is 3-7: 100.
The invention has the following beneficial effects:
(1) The invention adopts a coating method to ensure that the paper has the characteristics of hydrophobicity and flame retardance, and has the characteristics of simple and easily obtained operation and equipment, easy industrialized mass production and the like.
(2) The water contact angle of melamine cyanurate before and after hydrophobic modification by the sol-gel method is improved from 32.6 degrees to 127.3 degrees, the water contact angle of aluminum hydroxide before and after modification is improved from 38.3 degrees to 126.1 degrees, and the sol-gel method converts the hydrophilicity of the flame retardant into the hydrophobicity, so that the flame retardant is not separated out on the surface of paper due to moisture absorption, and the physical performance and the flame retardant effect of the paper are reduced.
(3) The Cobb value of the hydrophobic flame-retardant paper is 26.1g/m 2 LOI is 30.2%, and the flame retardant has good hydrophobic flame retardant property.
Drawings
FIG. 1 relationship between the amount of silane coupling agent used and the contact angles of melamine cyanurate and aluminum hydroxide
FIG. 2 LOI values of different hydrophobic flame retardant coating formulations and paper
FIG. 3 different hydrophobic flame retardant coating formulations versus the Cobb value of the paper.
Detailed Description
The technical solutions of the present invention will be fully described below with reference to specific embodiments of the present invention, which are only a part of the embodiments of the present invention, but not all of them. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
1. The first embodiment.
The method for preparing the hydrophobic flame-retardant paper by coating comprises the following steps:
1. preparing the hydrophobic modified flame retardant by a sol-gel method. Pouring 100g of ethanol and 100g of deionized water into a three-neck flask at 40 ℃ and stirring for 10 minutes by using a stirrer; then 50g of melamine cyanurate is added and stirred for 15 minutes; then sequentially adding 1g of surfactant OP-10 and 17g of ammonia water and stirring for at least 20 minutes; then, 8g of tetraethoxysilane is slowly dripped into the reaction system by using a constant-pressure dropping funnel and stirred for 10 minutes; then 1g of silane coupling agent is dripped to react for 4 hours; and finally, cooling the product to room temperature, filtering, washing with water and absolute ethyl alcohol respectively twice, and drying at 80 ℃ to obtain the hydrophobic modified flame retardant.
2. And (3) preparing the hydrophobic flame-retardant coating. The mass ratio of the melamine cyanurate to the aluminum hydroxide in the hydrophobic modified flame retardant is 4: 6, the modified flame retardant and the styrene-acrylic emulsion are mixed in a certain ratio, and the addition amount of the modified flame retardant accounts for 50% of the total mass of the hydrophobic flame retardant coating.
3. The hydrophobic flame-retardant paper is prepared by a coating method. And (3) coating the solid content of the hydrophobic flame-retardant coating on the base paper by 8 percent relative to the mass of the base paper, drying the coated paper at 105 ℃ for 30 minutes, heating to 160 ℃ for curing for 10 minutes, and cooling to room temperature to obtain the hydrophobic flame-retardant paper.
Through detection, the water contact angle of the hydrophobic modified melamine cyanurate prepared in the embodiment is 93.9 degrees, and the hydrophobic modified melamine cyanurate is hydrophobicThe water contact angle of the water modified aluminum hydroxide is 89.2 degrees; the Cobb value of the hydrophobic flame-retardant paper is 44.7g/m 2 LOI is 26.1%.
2. Example two.
The method for preparing the hydrophobic flame-retardant paper by coating comprises the following steps:
1. preparing the hydrophobic modified flame retardant by a sol-gel method. Pouring 100g of ethanol and 100g of deionized water into a three-neck flask at 30 ℃, and stirring for 10 minutes by using a stirrer; then 50g of melamine cyanurate is added and stirred for 15 minutes; then sequentially adding 1g of surfactant OP-10 and 17g of ammonia water and stirring for at least 20 minutes; then, 8g of tetraethoxysilane is slowly dripped into the reaction system by using a constant-pressure dropping funnel and stirred for 10 minutes; then 2g of silane coupling agent is dripped to react for 4 hours; and finally, cooling the product to room temperature, filtering, washing with water and absolute ethyl alcohol respectively twice, and drying at 80 ℃ to obtain the hydrophobic modified flame retardant.
2. And (3) preparing the hydrophobic flame-retardant coating. The mass ratio of the melamine cyanurate to the aluminum hydroxide in the hydrophobic modified flame retardant is 5: 5, the modified flame retardant is mixed with the styrene-acrylic emulsion in a certain ratio, and the addition amount of the modified flame retardant accounts for 55% of the total mass of the hydrophobic flame retardant coating.
3. The hydrophobic flame-retardant paper is prepared by a coating method. The solid content of the hydrophobic flame-retardant coating is 14 percent relative to the mass of the base paper, then the coated paper is dried at 105 ℃ for 30 minutes, heated to 160 ℃ for solidification for 10 minutes, and cooled to room temperature, thus obtaining the hydrophobic flame-retardant paper.
Through detection, the water contact angle of the hydrophobic modified melamine cyanurate prepared by the method is 121.5 degrees, and the water contact angle of the hydrophobic modified aluminum hydroxide is 117.7 degrees; the Cobb value of the hydrophobic flame-retardant paper is 32.6g/m 2 LOI is 27.7%.
3. Example three.
The method for preparing the hydrophobic flame-retardant paper by coating comprises the following steps:
1. preparing the hydrophobic modified flame retardant by a sol-gel method. Pouring 100g of ethanol and 100g of deionized water into a three-neck flask at 40 ℃ and stirring for 10 minutes by using a stirrer; then 50g of melamine cyanurate is added and stirred for 15 minutes; then, 1g of surfactant OP-10 and 17g of ammonia water are added in sequence and stirred for at least 20 minutes; then, 8g of tetraethoxysilane is slowly dripped into the reaction system by using a constant-pressure dropping funnel and stirred for 10 minutes; then 3g of silane coupling agent is dripped to react for 4 hours; and finally, cooling the product to room temperature, filtering, washing with water and absolute ethyl alcohol respectively twice, and drying at 80 ℃ to obtain the hydrophobic modified flame retardant.
2. And (3) preparing the hydrophobic flame-retardant coating. The mass ratio of the melamine cyanurate to the aluminum hydroxide in the hydrophobic modified flame retardant is 6: 4, the modified flame retardant and the styrene-acrylic emulsion are mixed in a certain ratio, and the addition amount of the modified flame retardant accounts for 60% of the total mass of the hydrophobic flame retardant coating.
3. The hydrophobic flame-retardant paper is prepared by a coating method. The solid content of the hydrophobic flame-retardant coating is 14 percent relative to the mass of the base paper, then the coated paper is dried at 105 ℃ for 30 minutes, heated to 160 ℃ for solidification for 10 minutes, and cooled to room temperature, thus obtaining the hydrophobic flame-retardant paper.
Through detection, the water contact angle of the hydrophobic modified melamine cyanurate prepared by the method is 127.3 degrees, and the water contact angle of the hydrophobic modified aluminum hydroxide is 126.1 degrees; the Cobb value of the hydrophobic flame-retardant paper is 26.4g/m 2 LOI is 28.6%.
4. Example four.
The method for preparing the hydrophobic flame-retardant paper by coating comprises the following steps:
1. preparing the hydrophobic modified flame retardant by a sol-gel method. Pouring 100g of ethanol and 100g of deionized water into a three-neck flask at 40 ℃ and stirring for 10 minutes by using a stirrer; then 50g of melamine cyanurate is added and stirred for 15 minutes; then, 1g of surfactant OP-10 and 17g of ammonia water are added in sequence and stirred for at least 20 minutes; then, 8g of tetraethoxysilane is slowly dripped into the reaction system by using a constant-pressure dropping funnel and stirred for 10 minutes; then 3g of silane coupling agent is dripped to react for 4 hours; and finally, cooling the product to room temperature, filtering, washing with water and absolute ethyl alcohol respectively twice, and drying at 80 ℃ to obtain the hydrophobic modified flame retardant.
2. And (3) preparing the hydrophobic flame-retardant coating. The mass ratio of the melamine cyanurate to the aluminum hydroxide in the hydrophobic modified flame retardant is 6: 4, the modified flame retardant and the styrene-acrylic emulsion are mixed in a certain ratio, and the addition amount of the modified flame retardant accounts for 65% of the total mass of the hydrophobic flame retardant coating.
3. Preparing hydrophobic flame-retardant paper by a coating method. Coating the hydrophobic flame-retardant coating on the base paper by 16 percent of the mass of the base paper, drying the coated paper at 105 ℃ for 30 minutes, heating to 160 ℃ for curing for 10 minutes, and cooling to room temperature to obtain the hydrophobic flame-retardant paper.
Through detection, the water contact angle of the hydrophobic modified melamine cyanurate prepared by the method is 127.3 degrees, and the water contact angle of the hydrophobic modified aluminum hydroxide is 126.1 degrees; the Cobb value of the hydrophobic flame-retardant paper is 26.1g/m 2 LOI is 30.2%.
Claims (4)
1. A method for preparing hydrophobic flame-retardant paper by coating is characterized by comprising the following steps:
(1) Preparing a hydrophobic modified flame retardant by a sol-gel method; pouring ethanol and deionized water in a certain proportion into a three-neck flask at the temperature of 30-50 ℃, and uniformly stirring by using a stirrer to obtain an ethanol solution; adding 50g of fire retardant into 200g of ethanol solution, and uniformly stirring; sequentially adding a surfactant OP-10 and ammonia water, and uniformly stirring; slowly dropwise adding tetraethoxysilane into a reaction system, uniformly stirring and fully reacting; then, dripping a silane coupling agent for reaction for 3 to 5 hours; finally, cooling the product to room temperature, filtering, washing with water and absolute ethyl alcohol respectively twice, and drying at 80 ℃ to obtain the hydrophobic modified flame retardant;
(2) Preparing a hydrophobic flame-retardant coating; mixing the hydrophobic modified flame retardant and the styrene-acrylic emulsion in a certain proportion, wherein the addition amount of the hydrophobic modified flame retardant accounts for 50-65% of the total mass of the hydrophobic flame-retardant coating;
(3) Preparing hydrophobic flame-retardant paper by a coating method; coating the base paper with the coating amount of the hydrophobic flame-retardant coating being 8-16% of the mass of the base paper, drying the coated paper at 105 ℃ for 30 minutes, heating to 160 ℃ for curing for 10 minutes, and cooling to room temperature to obtain the hydrophobic flame-retardant paper.
2. The method for preparing the hydrophobic flame-retardant paper by coating according to claim 1, wherein the volume ratio of the absolute ethyl alcohol to the deionized water in the step (1) is 1-2: 1, and the volume ratio of the ammonia water to the whole solvent system is 6-9: 100; the mass ratio of the ethyl orthosilicate to the flame retardant is 0.6-1: 5.
3. The method for preparing the hydrophobic flame-retardant paper by coating according to claim 1, wherein the flame retardant in the step (1) is melamine cyanurate and aluminum hydroxide, and the mass ratio is 4-6: 6-4.
4. The method for preparing hydrophobic flame-retardant paper by coating according to claim 1, wherein the silane coupling agent in step (1) is one or two of n-octyl triethoxysilane, ethyl triethoxysilane and gamma-methacryloxypropyl trimethoxysilane, and the mass ratio of the silane coupling agent to the flame retardant is 3-7: 100.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116163155A (en) * | 2023-02-14 | 2023-05-26 | 浙江理工大学 | Method for preparing hydrophobic flame-retardant paper by adding in pulp |
Citations (5)
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|---|---|---|---|---|
| JPH05194876A (en) * | 1991-08-05 | 1993-08-03 | Atom Chem Paint Co Ltd | Flame-retarding coating material |
| JP2001294763A (en) * | 2000-02-09 | 2001-10-23 | Ishizuka Glass Co Ltd | Method for manufacturing composite composition for giving flame retardance and composite composition for giving flame resistance |
| CN103805056A (en) * | 2012-11-15 | 2014-05-21 | 中国科学院合肥物质科学研究院 | Nanometer fire retardant coating and preparation method thereof |
| CN110130148A (en) * | 2019-05-20 | 2019-08-16 | 陈莉玲 | A kind of preparation method of fire retardant papers |
| EP3951049A1 (en) * | 2020-06-24 | 2022-02-09 | Zhejiang Rongsheng Environmental Protection Paper Co., Ltd. | High-performance environment-friendly kraft liner board, and preparation method thereof |
-
2022
- 2022-05-30 CN CN202210597051.1A patent/CN115216993A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05194876A (en) * | 1991-08-05 | 1993-08-03 | Atom Chem Paint Co Ltd | Flame-retarding coating material |
| JP2001294763A (en) * | 2000-02-09 | 2001-10-23 | Ishizuka Glass Co Ltd | Method for manufacturing composite composition for giving flame retardance and composite composition for giving flame resistance |
| CN103805056A (en) * | 2012-11-15 | 2014-05-21 | 中国科学院合肥物质科学研究院 | Nanometer fire retardant coating and preparation method thereof |
| CN110130148A (en) * | 2019-05-20 | 2019-08-16 | 陈莉玲 | A kind of preparation method of fire retardant papers |
| EP3951049A1 (en) * | 2020-06-24 | 2022-02-09 | Zhejiang Rongsheng Environmental Protection Paper Co., Ltd. | High-performance environment-friendly kraft liner board, and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| 刘一山: "制浆造纸助剂及其应用技术", vol. 1, 中国轻工业出版社, pages: 106 - 108 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116163155A (en) * | 2023-02-14 | 2023-05-26 | 浙江理工大学 | Method for preparing hydrophobic flame-retardant paper by adding in pulp |
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