CN110318286A - A kind of preparation method of Halogen sound-absorbing and flame-retardant paper - Google Patents

Abstract

A kind of preparation method of Halogen sound-absorbing and flame-retardant paper, include the following steps: the selection of slurry, defibrination, plant fiber fabricated in situ inorganic fire retardants, it is with slurry, manufacture paper with pulp, impregnate, drying.The slurry of the Halogen sound-absorbing and flame-retardant paper includes 40%~70% softwood pulp, and the beating degree of needlebush is 20~35 ° of SR, 30%~60% glass fibre, the poly-vinyl alcohol solution that mass concentration is 5%~20%.The present invention combines a kind of green of various measures preparation, environmentally friendly and sound-absorbing and excellent fireproof performance Halogen sound-absorbing and flame-retardant paper, new decorative material for building is met for the feature of environmental protection, dicoration, the requirements at the higher level of anti-flammability, the conventional porous sound-absorbing material using centrifugally glass-wool as representative can be substituted, the improvement of noise pollution is also had a very important significance.

Description

A kind of preparation method of halogen-free sound-absorbing flame-retardant paper

technical field

The invention relates to the field of special paper-based functional materials, in particular to a preparation method of halogen-free sound-absorbing and flame-retardant paper.

Background technique

Noise pollution is a major public hazard to the human living environment. It not only seriously damages our auditory nerves, cardiovascular system and nervous system, but also accelerates the aging of buildings and industrial machinery, affecting the precision and service life of instruments. As everyone pays more and more attention to the problem of noise control, various methods of sound absorption and noise reduction have also been born. However, the traditional sound-absorbing material-glass wool has many defects, such as low noise reduction coefficient, short service life, non-environmental protection, and easy to cause secondary pollution. material replaced. Fiber-based sound-absorbing materials can have good sound-absorbing effects in a wide frequency band, so they can replace traditional porous sound-absorbing materials represented by centrifugal glass wool, which are environmentally friendly, reusable, decorative, and Sound-absorbing materials with superior acoustic performance will be more and more recognized by the market.

On the other hand, with the increasing requirements for practical life and fire safety, people have higher and higher requirements for flame retardancy of paper-based products. Most of the flame retardants currently used contain halogens, although their flame retardant efficiency is very high. However, a large amount of hydrogen halide gas will be released during combustion, producing thick smoke, causing secondary pollution, and causing harm to the human respiratory tract and other organs, and even threatening the safety of human life. At present, flame retardant technology has entered a new stage of development, and the flame retardant technology of paper-based materials in the future is developing in the direction of high efficiency, economy and environmental protection. Due to the advantages of inorganic flame retardants: low toxicity, good thermal stability; no precipitation, durable flame retardant effect; no corrosive gas; low price; The application of organic flame retardants is gradually replacing organic flame retardants, especially halogenated flame retardants, so the research on the synthesis of inorganic flame retardants is of great significance.

At present, the society's demand for sound-absorbing materials is growing rapidly, and traditional sound-absorbing materials can no longer meet people's higher requirements for environmental protection, decoration, and flame retardancy. Therefore, the research and development of new environmentally friendly sound-absorbing and flame-retardant materials has become the direction of efforts.

Contents of the invention

The purpose of the present invention is to provide a product that not only has a simple preparation process and excellent product performance, but also can meet the higher requirements of new building decoration materials for environmental protection, decoration, and flame retardancy, and is also very important for the control of noise pollution. A preparation method of halogen-free sound-absorbing and flame-retardant paper.

In order to achieve the above object, the technical scheme adopted in the present invention is:

1) Refining: taking coniferous wood pulp boards soaked in water, pre-refined, wringing out the pulp, and balancing moisture to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: Add magnesium chloride solution with a concentration of 0.5-1.5mol/L to softwood pulp, stir and pre-soak, then add sodium hydroxide solution to it for reaction, take out the slurry, and filter , wring out, and balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) Fiber dispersion: take 40% to 70% of coniferous wood pulp and 30% to 60% of glass fiber according to the mass percentage, put them in a deflaking machine, add water and 0.008% to 0.01% of the fiber mass dispersant, and decompose for 1w to obtain glass Mixed pulp of fibers and plant fibers;

4) Polyvinyl alcohol fiber dissolution: dissolve the polyvinyl alcohol fiber in water to make a polyvinyl alcohol solution with a mass concentration of 5% to 20%, add the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and use The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) Paper making: add 0.1% to 0.5% of its mass retention aid to the fiber mixed slurry, and then make paper on a paper sample machine;

6) Microwave drying: the wet paper web obtained by papermaking is placed in a microwave oven on high heat and microwave dried;

7) Drying: put the paper into a hot air circulation drying oven to dry to obtain a halogen-free sound-absorbing and flame-retardant paper.

Said step 1) The coniferous wood pulp board is soaked in water for more than 4 hours, the beating degree is 20-35°SR by using a PFI refiner, and the pulp equilibrium moisture time is at least 24 hours.

In the step 2) the slurry is presoaked in the magnesium chloride solution for 30-60 minutes, and the reaction time is 10-30 minutes.

The dispersant in step 3) is fatty amine oxide or polyethylene oxide.

The water melting temperature of the polyvinyl alcohol fiber in the step 4) is 70-90°C.

The retention aid in step 5) is a cationic retention aid, and the basis weight of the sheet formed by papermaking is 60-70 g/m ² .

The microwave drying time of the step 6) is 10-60s.

Step 6) The paper web after microwave drying is transferred between two copper nets, and the paper web is immersed in a flame retardant solution with a mass concentration of 0.5% to 3%.

The flame retardant is an organic flame retardant or a mixed flame retardant compounded by an inorganic flame retardant and an organic flame retardant in a mass ratio of 5:1-3, wherein the organic flame retardant is a phosphorus-nitrogen flame retardant, The inorganic flame retardant is magnesium hydroxide.

The step 8) drying temperature is 140°C-160°C.

The beneficial effects of the present invention are:

Firstly, the present invention exposes more free hydroxyl groups on the surface of the plant fibers by pretreating the plant fibers, thereby increasing the degree of fibrillation and water absorption swelling of the plant fibers. And the fiber cell filling technology is adopted, and magnesium chloride and sodium hydroxide are selected to react in the cell cavity or cell wall of the plant fiber, and the inorganic magnesium hydroxide flame retardant that generates a flame-retardant precipitate or sol in situ achieves the flame-retardant improvement of the plant fiber. For the purpose of improving the retention rate of magnesium hydroxide by adding cationic retention aids, and then further preparing flame-retardant paper.

Secondly, glass fiber is a high-performance fiber with light weight, high strength, non-combustibility, heat insulation and sound absorption. The product uses polyvinyl alcohol fiber as a binder, and mixes glass fiber and plant fiber through wet papermaking technology. A small amount of organic flame retardant can achieve the effect of organic and inorganic synergistic flame retardancy. The addition of glass fiber can improve the flame retardant performance of the paper on the one hand, on the other hand, the paper can still maintain its shape after burning, so that it will not float in the air and cause harm to the human body.

Finally, sound-absorbing materials with a single fiber component often cannot meet high sound-absorbing requirements, especially the sound-absorbing performance in the middle and low frequency bands. Halogen-free sound-absorbing and flame-retardant paper is a fiber-based porous sound-absorbing composite material, which can efficiently absorb broadband noise and conform to the development trend of green, light and high-efficiency sound-absorbing materials.

Detailed ways

The present invention will be described in further detail below in conjunction with specific examples, but not as a limitation of the present invention.

Example 1:

1) Refining: Soak coniferous wood pulp boards in water for more than 4 hours, then use a PFI refiner for pre-refining, control the degree of beating to 24°SR, wring out the pulp, and balance the water for more than 24 hours to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: Add magnesium chloride solution with a concentration of 0.5mol/L to the coniferous wood pulp, stir and pre-soak for 30 minutes, then add sodium hydroxide solution to it and react for 20 minutes, take out the slurry, and filter , wring out, and balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) fiber dispersion: get 70% coniferous wood pulp and 30% glass fiber by mass percentage and place it in the deflagging machine, add water and fiber quality 0.009% dispersant fatty amine oxide, decompose 1w and turn to obtain glass fiber and plant fiber mixed slurry;

4) Dissolving polyvinyl alcohol fibers: dissolving polyvinyl alcohol fibers in water at 70°C to form a polyvinyl alcohol solution with a mass concentration of 10%, adding the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and using The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) copying: after adding its mass 0.5% cationic retention aid to the fiber mixed slurry, copying and forming on the paper sample machine;

6) Microwave drying: place the wet paper web obtained by papermaking in a microwave oven on high heat and microwave dry for 60s;

7) Drying: put the paper into a hot air circulation drying oven and dry at 140°C to obtain a halogen-free sound-absorbing and flame-retardant paper.

The halogen-free sound-absorbing and flame-retardant paper prepared according to the method described in this example has a basis weight of 60 g/m ² , a bulk thickness of 4.33 cm ³ /g, a tensile strength of 20.5 N/15 mm, and a synthetic content of magnesium hydroxide of 20 %, the carbonization length of the paper is 86mm, the second-grade flame retardant, and the average sound absorption coefficient can reach 0.47.

Example 2:

1) Refining: Soak coniferous wood pulp boards in water for more than 4 hours, then use a PFI refiner for pre-refining, control the degree of beating to 24°SR, wring out the pulp, and balance the water for more than 24 hours to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: Add magnesium chloride solution with a concentration of 0.5mol/L to the coniferous wood pulp, stir and pre-soak for 50 minutes, then add sodium hydroxide solution to it and react for 10 minutes, take out the slurry, and filter , wring out, and balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) Fiber dispersion: take 40% coniferous wood pulp and 60% glass fiber by mass percentage and place it in a deflaking machine, add water and fiber quality 0.008% dispersant polyethylene oxide, and decompose for 1w to obtain a mixture of glass fiber and plant fiber slurry;

4) Dissolving polyvinyl alcohol fibers: dissolving polyvinyl alcohol fibers in water at 90°C to form a polyvinyl alcohol solution with a mass concentration of 10%, adding the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and using The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) copying: after adding its mass 0.5% cationic retention aid to the fiber mixed slurry, copying and forming on the paper sample machine;

6) Microwave drying: place the wet paper web obtained by papermaking in a microwave oven on high heat and microwave dry for 60s;

7) Drying: put the paper into a hot air circulation drying oven and dry at 150°C to obtain a halogen-free sound-absorbing and flame-retardant paper.

The halogen-free sound-absorbing and flame-retardant paper prepared by the method of the present invention has a basis weight of 60g/m ² , a bulk thickness of 4.39cm ³ /g, a tensile strength of 16.8 N/15mm, and a synthetic content of magnesium hydroxide of 30%. , the carbonization length of the paper is 77mm, the second-grade flame retardant, and the average sound absorption coefficient can reach 0.49.

Example 3:

1) Refining: Soak coniferous wood pulp boards in water for more than 4 hours, then use PFI refiner for refining pretreatment, control the degree of beating to 30°SR, wring out the pulp, and balance the water for more than 24 hours to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: adding a magnesium chloride solution with a concentration of 1mol/L to the coniferous wood pulp, stirring, and pre-soaking for 50 minutes, then adding sodium hydroxide solution to it and reacting for 10 minutes, then taking out the slurry, filtering, Wring out, balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) fiber dispersion: get 60% coniferous wood pulp and 40% glass fiber by mass percentage and place it in the disintegrating machine, add water and fiber quality 0.01% dispersant fatty amine oxide, disintegrate 1w and turn to obtain glass fiber and plant fiber mixed slurry;

4) Polyvinyl alcohol fiber dissolving: dissolving the polyvinyl alcohol fiber in water at 80°C to form a polyvinyl alcohol solution with a mass concentration of 10%, adding the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and using The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) copying: after adding its mass 0.5% cationic retention aid to the fiber mixed slurry, copying and forming on the paper sample machine;

6) Microwave drying: place the wet paper web obtained by papermaking in a microwave oven on high heat and microwave dry for 60s;

7) Impregnation: transfer the microwave-dried paper web between two copper nets, and immerse the paper web in a phosphorus-nitrogen flame retardant solution with a mass concentration of 0.5%;

8) Drying: put the paper into a hot air circulation drying oven and dry at 160°C to obtain a halogen-free sound-absorbing and flame-retardant paper.

The halogen-free sound-absorbing and flame-retardant paper prepared by the method of the present invention has a basis weight of 60g/m ² , a bulk thickness of 4.48cm ³ /g, a tensile strength of 19.8 N/15mm, and a synthetic content of magnesium hydroxide of 30%. , the mass concentration of the impregnating liquid is 0.5%, and when the impregnating time is 60s, the carbonization length of the paper is 64mm, the grade 2 flame retardant, and the average sound absorption coefficient can reach 0.56.

Example 4:

1) Refining: Soak coniferous wood pulp boards in water for more than 4 hours, then use a PFI refiner for pre-refining, control the beating degree to 30°SR, wring out the pulp, and balance the water for more than 24 hours to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: Add magnesium chloride solution with a concentration of 1.5mol/L to the coniferous wood pulp, stir and pre-soak for 60 minutes, then add sodium hydroxide solution to it and react for 30 minutes, take out the slurry, and filter , wring out, and balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) Fiber dispersion: take 50% coniferous wood pulp and 50% glass fiber by mass percentage and place it in a deflaking machine, add water and fiber quality 0.0085% dispersant polyethylene oxide, and decompose for 1w to obtain a mixture of glass fiber and plant fiber slurry;

4) Polyvinyl alcohol fiber dissolution: dissolve the polyvinyl alcohol fiber in water at 75°C to form a polyvinyl alcohol solution with a mass concentration of 20%, add the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and use The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) Paper making: after adding 0.1% of its mass cationic retention aid to the fiber mixed slurry, it is made on a paper sample machine;

6) Microwave drying: place the wet paper web obtained by papermaking in a microwave oven on high heat and microwave dry for 10s;

7) Impregnation: transfer the microwave-dried paper web between two copper nets, and immerse the paper web in a phosphorus-nitrogen flame retardant solution with a mass concentration of 1%;

8) Drying: put the paper into a hot air circulation drying oven and dry at 145°C to obtain a halogen-free sound-absorbing and flame-retardant paper.

The halogen-free sound-absorbing and flame-retardant paper prepared by the method of the present invention has a basis weight of 60g/m ² , a bulk thickness of 4.40cm ³ /g, a tensile strength of 17.6N/15mm, and a synthetic content of magnesium hydroxide of 30%. , when the impregnating liquid concentration is 1%, and when the impregnating time is 60s, the carbonization length of the paper is 48mm, the first-class flame retardant, and the average sound absorption coefficient can reach 0.50.

Example 5:

1) Refining: Soak coniferous wood pulp boards in water for more than 4 hours, then use PFI refiner for refining pretreatment, control the degree of beating to 35°SR, wring out the pulp, and balance the water for more than 24 hours to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: adding a magnesium chloride solution with a concentration of 1mol/L to the coniferous wood pulp, stirring, and pre-soaking for 40 minutes, then adding sodium hydroxide solution to it and reacting for 10 minutes, then taking out the slurry, filtering, Wring out, balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) fiber dispersion: get 65% coniferous wood pulp and 35% glass fibers by mass percentage and place them in a disintegrating machine, add water and fiber quality 0.0095% dispersant fatty amine oxide, disintegrate 1w and turn to obtain glass fibers and plant fibers mixed slurry;

4) Dissolving polyvinyl alcohol fibers: dissolving polyvinyl alcohol fibers in water at 85°C to form a polyvinyl alcohol solution with a mass concentration of 5%, adding the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and using The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) copying: after adding its quality 0.3% cationic retention aid to the fiber mixed slurry, copying and forming on the paper sample machine;

6) Microwave drying: place the wet paper web obtained by papermaking in a microwave oven on high heat and microwave dry for 30s;

7) Impregnation: transfer the microwave-dried paper web between two copper nets, and impregnate the paper web in a compound of phosphorus-nitrogen flame retardant with a mass concentration of 2% and magnesium hydroxide in a mass ratio of 5:1 In the mixed flame retardant solution;

8) Drying: put the paper into a hot air circulation drying oven and dry at 155°C to obtain a halogen-free sound-absorbing and flame-retardant paper.

The halogen-free sound-absorbing and flame-retardant paper prepared by the method of the present invention has a quantitative value of 60g/m2, a bulk thickness of ^4.43cm3 /g, a tensile strength of 17.6N/15mm, and a magnesium hydroxide synthesis amount of 30%. , When the impregnating solution concentration is 2%, when the impregnating time is 60s, the carbonization length of the paper is 25mm, the first-class flame retardant, and the average sound absorption coefficient can reach 0.53.

Embodiment 6:

1) Refining: Soak coniferous wood pulp boards in water for more than 4 hours, then use PFI refiner for refining pretreatment, control the degree of beating to 20°SR, wring out the pulp, and balance the water for more than 24 hours to obtain coniferous wood pulp;

2) In-situ synthesis of magnesium hydroxide by plant fibers: Add magnesium chloride solution with a concentration of 1.2mol/L to the coniferous wood pulp, stir and pre-soak for 50 minutes, then add sodium hydroxide solution to it and react for 25 minutes, take out the slurry, and filter , wring out, and balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2;

3) Fiber dispersion: take 70% coniferous wood pulp and 30% glass fibers by mass percentage and place them in a deflaking machine, add water and fiber quality 0.01% dispersant polyethylene oxide, and decompose for 1w to obtain a mixture of glass fibers and plant fibers slurry;

4) Dissolving polyvinyl alcohol fibers: dissolving polyvinyl alcohol fibers in water at 80°C to form a polyvinyl alcohol solution with a mass concentration of 15%, adding the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and using The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry;

5) copying: after adding its mass 0.4% cationic retention aid to the fiber mixed slurry, copying and forming on the paper sample machine;

6) Microwave drying: place the wet paper web obtained by papermaking in a microwave oven on high heat and microwave dry for 40s;

7) Impregnation: Transfer the microwave-dried paper web between two copper nets, and impregnate the paper web in a compound of phosphorus-nitrogen flame retardant with a mass concentration of 3% and magnesium hydroxide in a mass ratio of 5:3 In the mixed flame retardant solution;

8) Drying: put the paper into a hot air circulation drying oven and dry at 160°C to obtain a halogen-free sound-absorbing and flame-retardant paper.

Claims (10)

1. A preparation method of halogen-free sound-absorbing flame-retardant paper, characterized in that, comprising the following steps: 1) Refining: taking coniferous wood pulp boards soaked in water, pre-refined, wringing out the pulp, and balancing moisture to obtain coniferous wood pulp; 2) In-situ synthesis of magnesium hydroxide by plant fibers: Add magnesium chloride solution with a concentration of 0.5-1.5mol/L to softwood pulp, stir and pre-soak, then add sodium hydroxide solution to it for reaction, take out the slurry, and filter , wring out, and balance moisture to obtain softwood pulp, wherein the molar concentration ratio of magnesium chloride solution and sodium hydroxide solution is 1:2; 3) Fiber dispersion: take 40% to 70% of coniferous wood pulp and 30% to 60% of glass fiber according to the mass percentage, put them in a deflaking machine, add water and 0.008% to 0.01% of the fiber mass dispersant, and decompose for 1w to obtain glass Mixed pulp of fibers and plant fibers; 4) Polyvinyl alcohol fiber dissolution: dissolve the polyvinyl alcohol fiber in water to make a polyvinyl alcohol solution with a mass concentration of 5% to 20%, add the mixed slurry to the polyvinyl alcohol solution at a concentration of 0.1%, and use The glass rod is stirred and dispersed into a uniformly suspended fiber mixed slurry; 5) Paper making: add 0.1% to 0.5% of its mass retention aid to the fiber mixed slurry, and then make paper on a paper sample machine; 6) Microwave drying: the wet paper web obtained by papermaking is placed in a microwave oven on high heat and microwave dried; 7) Drying: put the paper into a hot air circulation drying oven to dry to obtain a halogen-free sound-absorbing and flame-retardant paper. 2. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that, the step 1) soaking time of the coniferous wood pulp board in water is more than 4 hours, and the degree of beating by using a PFI refiner is 20-2. 35 ° SR, the slurry balance moisture time is at least 24h. 3. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that in step 2) the slurry is presoaked in magnesium chloride solution for 30-60 minutes, and the reaction time is 10-30 minutes. 4. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that: the dispersant in step 3) is aliphatic amine oxide or polyethylene oxide. 5. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that: in the step 4), the water melting temperature of the polyvinyl alcohol fiber is 70-90°C. 6. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that: the retention aid in the step 5) is a cationic retention aid, and the weight of paper sheets formed by copying is 60-70g/ m ² . 7. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that: the microwave drying time of the step 6) is 10-60s. 8. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that: said step 6) the paper web after microwave drying is transferred between two copper nets, and the paper web is immersed in a mass A flame retardant solution with a concentration of 0.5% to 3%. 9. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 8, characterized in that: the flame retardant is an organic flame retardant or an inorganic flame retardant and an organic flame retardant according to the ratio of 5:1-3 The mixed flame retardant compounded by mass ratio, wherein the organic flame retardant is phosphorus nitrogen flame retardant, and the inorganic flame retardant is magnesium hydroxide. 10. The preparation method of halogen-free sound-absorbing and flame-retardant paper according to claim 1, characterized in that: the drying temperature in step 8) is 140°C-160°C.