阅读说明：本技术 一种高阻燃隔热型喷胶棉的制备方法 (Preparation method of high-flame-retardant heat-insulation type glue-sprayed cotton ) 是由 张彩 于 2020-07-08 设计创作，主要内容包括：本发明公开了一种高阻燃隔热型喷胶棉的制备方法,属于纺织品技术领域。本发明首先将蛭石、蒙脱土研磨,研磨后与甲苯混合制得混合物,向混合物中加入氯化钙混合,再滴加碱液混合制得预制浆液,随后将预制浆液浓缩干燥、高温处理制得热处理反应物,然后将甘蔗渣、秸秆混合,用盐酸浸泡,再滴加碱液高温处理制得反应浆液,将反应浆液调节pH值后与纤维素酶投入酶解罐中酶解制得酶解反应物,随后将酶解反应物与热处理反应物语混合,用乙醇浸泡进行高温高压反应制得改性粘结物,随后将改性粘结物喷洒于棉纤维上,最后将棉纤维干燥、热压、切边、打包制得高阻燃隔热型喷胶棉,隔热性能和保温性能增强,增强阻燃性能,降低透风率,使保温性能增强。(The invention discloses a preparation method of high-flame-retardant heat-insulation type glue-sprayed cotton, and belongs to the technical field of textiles. The invention firstly grinds vermiculite and montmorillonite, mixes the grinded vermiculite and montmorillonite with toluene to prepare a mixture, adds calcium chloride into the mixture to mix, then adds alkali liquor to mix to prepare prefabricated slurry, then concentrates, dries and treats the prefabricated slurry at high temperature to prepare a heat treatment reactant, then mixing bagasse and straw, soaking the mixture with hydrochloric acid, dropwise adding alkali liquor to perform high-temperature treatment to prepare reaction slurry, adjusting the pH value of the reaction slurry, putting the reaction slurry and cellulase into an enzymolysis tank for enzymolysis to prepare an enzymolysis reactant, then mixing the enzymolysis reactant with a heat treatment reactant, soaking the mixture with ethanol for high-temperature and high-pressure reaction to prepare a modified bonding material, then spraying the modified bonding material on cotton fibers, and finally drying, hot-pressing, trimming and packaging the cotton fibers to prepare the high-flame-retardant and heat-insulation type spray bonded cotton.)

1. A preparation method of high flame-retardant heat-insulation type glue-sprayed cotton is characterized by comprising the following specific preparation steps:

(1) putting an enzymolysis reactant and a heat treatment reactant into a reaction kettle, soaking the reactants in 20-25% of ethanol solution by mass, stirring the reactants at the rotating speed of 1100-1200 r/min by using a stirrer for 50-60 min to prepare dispersion, adding alkyd resin into the reaction kettle, uniformly stirring the mixture, sealing the reaction kettle after stirring, filling nitrogen into the reaction kettle, raising the pressure in the reaction kettle to 1.6-1.8 MPa, raising the temperature in the reaction kettle to 150-170 ℃, and reacting the mixture at constant temperature and constant pressure for 40-60 min to prepare a modified adhesive;

(2) spreading and carding cotton fibers, putting the cotton fibers into a glue spraying drying box, uniformly spraying modified bonding substances on the surfaces of the cotton fibers, putting the cotton fibers into a drying box with the temperature of 70-80 ℃ after spraying, standing for 60-80 min, putting the cotton fibers into a hot press for hot pressing after standing, and trimming and packaging after hot pressing to obtain the high-flame-retardant heat-insulation glue spraying cotton;

the specific preparation steps of the enzymolysis reactant are as follows:

(1) putting bagasse and crop straws into a beaker, soaking the beaker in 5-10% hydrochloric acid, putting the beaker into an ultrasonic oscillator, oscillating for 2-3 h under the condition of frequency of 32-36 kHz, dropwise adding 10-15% sodium hydroxide solution into the beaker to adjust the pH value to 9-10, putting the beaker into a resistance heating sleeve, raising the temperature in the heating sleeve to 105-110 ℃, and reacting at constant temperature for 130-150 min to prepare reaction slurry;

(2) putting the reaction slurry into a glass vessel, dropwise adding an acetic acid solution with the mass fraction of 5-10% into the glass vessel to adjust the pH value to 6.2-6.5 to prepare a reaction mixture, putting the reaction mixture and cellulase into an enzymolysis tank, sealing the enzymolysis tank, placing the enzymolysis tank in a greenhouse with the indoor temperature of 30-35 ℃, and standing at constant temperature for 20-24 hours to prepare an enzymolysis reactant;

the specific preparation steps of the heat treatment reactant are as follows:

(1) putting vermiculite and montmorillonite into a planetary ball mill, grinding for 80-100 min under the conditions that the rotating speed is 60-80 r/min and the ball-to-material ratio is 10:1 to obtain a grinding mixture, putting the grinding mixture and methylbenzene into a beaker, and stirring for 30-40 min by using a stirrer at the rotating speed of 300-400 r/min to obtain a mixture;

(2) adding calcium chloride powder with the mass of 1.0-1.5% of the mixture into a beaker, placing the beaker into a water bath kettle with the water bath temperature of 90-100 ℃, stirring for 50-60 min at the constant temperature by using a stirrer at the rotating speed of 500-600 r/min to prepare mixed slurry, and putting the mixed slurry and sodium hydroxide solution with the mass fraction of 3-5% into a reaction kettle to be uniformly mixed to prepare prefabricated slurry;

(3) putting the prefabricated slurry into a rotary evaporator, drying at the rotating speed of 120-160 r/min and the temperature of 110-120 ℃ until the quality of the product is constant to obtain a reaction product, putting the reaction product into an oven, drying at the temperature of 105-115 ℃ for 3-4 h, putting the reaction product into a muffle furnace after drying, raising the temperature in the muffle furnace to 700-800 ℃, standing at a constant temperature for 80-100 min, cooling, grinding and sieving with a 50-mesh sieve to obtain a heat treatment reactant.

2. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the mass ratio of the enzymolysis reactant to the heat treatment reactant is 1: 4.

3. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the mass of the alkyd resin added into the reaction kettle is 200-300% of the mass of the dispersion liquid.

4. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the mass of the sprayed modified bonding material is 15-20% of the mass of the cotton fiber.

5. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the mass ratio of the bagasse to the crop straw in the specific preparation step (1) of the enzymatic hydrolysis reactant is 10: 1.

6. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the mass ratio of the reaction mixture to the cellulase in the specific preparation step (2) of the enzymolysis reactant is 100: 1.

7. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the mass ratio of the vermiculite to the montmorillonite in the specific preparation step (1) of the heat treatment reactant is 5: 1.

8. The preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the specific preparation of the heat treatment reactant(s) the ground mixture described in step (1) and toluene are mixed in a mass ratio of 1: 5.

9. the preparation method of the high flame-retardant and heat-insulation type glue-sprayed cotton according to claim 1, characterized by comprising the following steps: the specific preparation step (2) of the heat treatment reactant is that the mass of the calcium chloride powder added into the beaker is 1.0-1.5% of the mass of the mixture, and the mass ratio of the mixed slurry to the sodium hydroxide solution with the mass fraction of 3-5% is 10: 1.

Technical Field

The invention discloses a preparation method of high-flame-retardant heat-insulation type glue-sprayed cotton, and belongs to the technical field of textiles.

Background

The bedding and clothing industry mainly adopts natural fibers, silk, wool, cotton wadding, camel hair, down feather and the like as middle filling materials. Along with the development of social demands, the raw materials such as cotton, down feather and the like are limited by resources, and the price is increasingly high. The natural raw materials also have some defects which are difficult to overcome, such as the cotton is easy to be affected with damp, the heat preservation and the air permeability are not stable enough, and the weight is obviously improved after being affected with damp; the down products are easy to be mildewed and damaged by moisture, and the feathers are easy to be drilled out of the fabric when the down products are worn, so that the wearing effect is influenced; in addition, the natural raw materials can not adapt to the industrial production of the clothing industry, the production period of ready-made clothes is long, and the cost is high. Therefore, the glue-sprayed cotton is taken as a novel wadding material and is produced.

The glue-spraying cotton is also called gunite cotton, which is a kind of non-woven fabric. It is made up by using natural cotton fibre, artificial fibre or synthetic fibre through the processes of loosening, carding, spraying glue, baking and curing. The principle of the formation of the collodion spraying structure is that the adhesive is sprayed on both sides of the fluffy fiber layer, because of certain pressure during spraying and suction force during vacuum liquid absorption at the lower part, the adhesive can be infiltrated into the interior of the fiber layer, and the fiber layer after being sprayed with the adhesive is dried and cured, so that the junction points between fibers are bonded, and the fibers which are not bonded with each other still have a great degree of freedom. Meanwhile, in the three-dimensional network structure, many air-containing voids remain. Therefore, the fiber layer has the warm keeping function of porosity and high bulkiness. Because of its fluffy, high compression resilience, dry and wet washing resistance, light weight and heat preservation, it has become an important material for processing and manufacturing bedding articles such as cotton clothes, ski wear, space suit, quilt, sleeping bag and some industrial articles in recent years.

The glue-sprayed cotton is sprayed with adhesive and is not soaked, and after spraying, it is no longer pressed by pressure and solidified. Therefore, in the bonded state of the fibers, the cross-point contact is more, and the adhesive bridges less clumps, which is the main reason why the cotton wool can keep loose, soft and warm.

Whereas the warmth retention of the spray bonded cotton increases linearly with the weight per unit area. The heat preservation performance of the spray-bonded cotton can be improved by increasing the quality of the spray-bonded cotton, but the air permeability and the air permeability of the spray-bonded cotton are greatly reduced, and the comfort is also reduced. Many scientific and technological workers start with the adhesive and try to solve the contradiction between the flexibility and the air permeability, but the contradiction is usually solved on the heat preservation performance only by increasing the gram weight of the glue-spraying cotton, and the hard requirement on the raw materials cannot be changed.

In recent years, the material has become one of the main raw materials for processing and manufacturing bedding articles such as cotton suits, space suits, quilts or sleeping bags and the like, even industrial articles. However, it can be seen that the above application scenarios also provide new requirements for various performance indexes of the collodion material, which mainly focus on the following points: due to the fact that the condition of high cold or strong wind exists in most use scenes, the product can keep out wind and keep warm for a long time only by needing the material to have low air permeability and low thermal conductivity; in addition, because the raw materials are flammable, the flame retardant property of the glue-sprayed cotton is required to be high, and the danger degree of the fire to the society is reduced.

Therefore, the invention of the spray-bonded cotton with good heat preservation, high air permeability and good flame retardance is necessary for the technical field of textiles.

Disclosure of Invention

The technical problems to be solved by the invention are as follows: aiming at the defects of poor heat insulation performance, high air permeability and poor flame retardant property of the current spray-bonded cotton, the preparation method of the high flame retardant and heat insulation type spray-bonded cotton is provided.

In order to solve the technical problems, the invention adopts the technical scheme that:

the preparation method of the high flame-retardant heat-insulation type glue-sprayed cotton comprises the following steps:

(1) putting an enzymolysis reactant and a heat treatment reactant into a reaction kettle, soaking the reactants in 20-25% of ethanol solution by mass, stirring the reactants at the rotating speed of 1100-1200 r/min by using a stirrer for 50-60 min to prepare dispersion, adding alkyd resin into the reaction kettle, uniformly stirring the mixture, sealing the reaction kettle after stirring, filling nitrogen into the reaction kettle, raising the pressure in the reaction kettle to 1.6-1.8 MPa, raising the temperature in the reaction kettle to 150-170 ℃, and reacting the mixture at constant temperature and constant pressure for 40-60 min to prepare a modified adhesive;

(2) spreading and carding cotton fibers, putting the cotton fibers into a glue spraying drying box, uniformly spraying modified bonding substances on the surfaces of the cotton fibers, putting the cotton fibers into a drying box with the temperature of 70-80 ℃ after spraying, standing for 60-80 min, putting the cotton fibers into a hot press for hot pressing after standing, and trimming and packaging after hot pressing to obtain the high-flame-retardant heat-insulation glue spraying cotton;

the specific preparation steps of the enzymolysis reactant are as follows:

(1) putting bagasse and crop straws into a beaker, soaking the beaker in 5-10% hydrochloric acid, putting the beaker into an ultrasonic oscillator, oscillating for 2-3 h under the condition of frequency of 32-36 kHz, dropwise adding 10-15% sodium hydroxide solution into the beaker to adjust the pH value to 9-10, putting the beaker into a resistance heating sleeve, raising the temperature in the heating sleeve to 105-110 ℃, and reacting at constant temperature for 130-150 min to prepare reaction slurry;

(2) putting the reaction slurry into a glass vessel, dropwise adding an acetic acid solution with the mass fraction of 5-10% into the glass vessel to adjust the pH value to 6.2-6.5 to prepare a reaction mixture, putting the reaction mixture and cellulase into an enzymolysis tank, sealing the enzymolysis tank, placing the enzymolysis tank in a greenhouse with the indoor temperature of 30-35 ℃, and standing at constant temperature for 20-24 hours to prepare an enzymolysis reactant;

the specific preparation steps of the heat treatment reactant are as follows:

(1) putting vermiculite and montmorillonite into a planetary ball mill, grinding for 80-100 min under the conditions that the rotating speed is 60-80 r/min and the ball-to-material ratio is 10:1 to obtain a grinding mixture, putting the grinding mixture and methylbenzene into a beaker, and stirring for 30-40 min by using a stirrer at the rotating speed of 300-400 r/min to obtain a mixture;

(2) adding calcium chloride powder with the mass of 1.0-1.5% of the mixture into a beaker, placing the beaker into a water bath kettle with the water bath temperature of 90-100 ℃, stirring for 50-60 min at the constant temperature by using a stirrer at the rotating speed of 500-600 r/min to prepare mixed slurry, and putting the mixed slurry and sodium hydroxide solution with the mass fraction of 3-5% into a reaction kettle to be uniformly mixed to prepare prefabricated slurry;

(3) putting the prefabricated slurry into a rotary evaporator, drying at the rotating speed of 120-160 r/min and the temperature of 110-120 ℃ until the quality of the product is constant to obtain a reaction product, putting the reaction product into an oven, drying at the temperature of 105-115 ℃ for 3-4 h, putting the reaction product into a muffle furnace after drying, raising the temperature in the muffle furnace to 700-800 ℃, standing at a constant temperature for 80-100 min, cooling, grinding and sieving with a 50-mesh sieve to obtain a heat treatment reactant.

The mass ratio of the enzymolysis reactant to the heat treatment reactant is 1: 4.

The mass of the alkyd resin added into the reaction kettle is 200-300% of the mass of the dispersion liquid.

The mass of the sprayed modified bonding material is 15-20% of the mass of the cotton fiber.

The mass ratio of the bagasse to the crop straw in the specific preparation step (1) of the enzymatic hydrolysis reactant is 10: 1.

The mass ratio of the reaction mixture to the cellulase in the specific preparation step (2) of the enzymolysis reactant is 100: 1.

The mass ratio of the vermiculite to the montmorillonite in the specific preparation step (1) of the heat treatment reactant is 5: 1.

The specific preparation of the heat treatment reactant(s) the ground mixture described in step (1) and toluene are mixed in a mass ratio of 1: 5.

the specific preparation step (2) of the heat treatment reactant is that the mass of the calcium chloride powder added into the beaker is 1.0-1.5% of the mass of the mixture, and the mass ratio of the mixed slurry to the sodium hydroxide solution with the mass fraction of 3-5% is 10: 1.

The beneficial technical effects of the invention are as follows:

(1) grinding vermiculite and montmorillonite, mixing the ground mixture with toluene to prepare a mixture, adding calcium chloride into the mixture for mixing, then adding alkali liquor dropwise for mixing to prepare prefabricated slurry, then concentrating, drying and carrying out high-temperature treatment on the prefabricated slurry to prepare a heat treatment reactant, then mixing bagasse and straw, soaking the bagasse and straw with hydrochloric acid, then adding alkali liquor dropwise for carrying out high-temperature treatment to prepare reaction slurry, adjusting the pH value of the reaction slurry, then putting the reaction slurry and cellulase into an enzymolysis tank for enzymolysis to prepare an enzymolysis reactant, then mixing the enzymolysis reactant and the heat treatment reactant, soaking the mixture with ethanol for carrying out high-temperature high-pressure reaction to prepare a modified bonding material, then spraying the modified bonding material on cotton fibers, and finally drying, hot-pressing, trimming and packaging the cotton fibers to prepare the high-flame-retardant heat-insulation type glue-spraying cotton. The expanded vermiculite contains a large number of pore structures, gas is introduced into the vermiculite, the thermal conductivity of the gas is very low, the heat insulation performance of the vermiculite structures is effectively improved, the vermiculite is adhered to the glue-spraying cotton and can enhance the heat insulation performance and the heat preservation performance of the glue-spraying cotton, the montmorillonite is hydrolyzed to a certain degree, metal ions in the montmorillonite are dissociated, the adsorption effect with the glue-spraying cotton is enhanced through mutual attraction of positive and negative charges, the metal ions are dispersed in the surface of vermiculite molecules and the fiber structure of the glue-spraying cotton and react with hydroxyl ions and high temperature to generate metal oxide molecules again, a gap structure in the glue-spraying cotton is filled, each component in the glue-spraying cotton is coated, the good flame retardant performance and the high temperature resistance of the glue-spraying cotton are combined, the flame retardant performance of the glue-spraying is effectively enhanced, and the air permeability of the glue-spraying cotton is reduced by filling the gaps, so that the;

(2) the method comprises the steps of soaking bagasse and straws in acid-alkali liquor, performing high-temperature high-pressure treatment, performing enzymolysis reaction and other modes to separate fibers, cellulose, cane sugar and other organic components in the bagasse and the straws, performing enzymolysis treatment on the cellulose by using cellulase, degrading the cellulose to generate micromolecular carbohydrate compounds, reinforcing the adsorption of the fiber components by using a large number of hydrogen bonds carried by the fiber components, forming a complex cross-linked network structure in the glue-sprayed cotton by the fiber components to reinforce the structural compactness of the glue-sprayed cotton, reduce the air permeability and enhance the heat preservation performance, adsorbing the structural strength of the fiber components by calcium ion calcium carbonate nanoparticles, filling gaps, further reducing the air permeability, improving the heat preservation performance and having wide application prospects.

Detailed Description

Putting vermiculite and montmorillonite into a planetary ball mill according to a mass ratio of 5:1, grinding for 80-100 min under the conditions that the rotating speed is 60-80 r/min and the ball-material ratio is 10:1 to prepare a grinding mixture, and mixing the grinding mixture and toluene according to a mass ratio of 1: 5, putting the mixture into a beaker, and stirring the mixture for 30 to 40min by a stirrer at the rotating speed of 300 to 400r/min to prepare a mixture; adding calcium chloride powder with the mass of 1.0-1.5% of the mixture into the beaker, placing the beaker into a water bath kettle with the water bath temperature of 90-100 ℃, stirring for 50-60 min at the constant temperature by using a stirrer at the rotating speed of 500-600 r/min to prepare mixed slurry, and putting the mixed slurry and sodium hydroxide solution with the mass fraction of 3-5% into a reaction kettle according to the mass ratio of 10:1 to uniformly mix to prepare prefabricated slurry; putting the prefabricated slurry into a rotary evaporator, drying at the rotating speed of 120-160 r/min and the temperature of 110-120 ℃ until the quality of the product is constant to obtain a reaction product, putting the reaction product into an oven, drying at the temperature of 105-115 ℃ for 3-4 hours, putting the reaction product into a muffle furnace after drying, raising the temperature in the muffle furnace to 700-800 ℃, standing at the constant temperature for 80-100 min, cooling, grinding and sieving with a 50-mesh sieve to obtain a heat treatment reactant for later use; putting bagasse and crop straws into a beaker according to a mass ratio of 10:1, soaking the beaker in 5-10% hydrochloric acid, putting the beaker into an ultrasonic oscillator, oscillating for 2-3 h under the condition of frequency of 32-36 kHz, dropwise adding 10-15% sodium hydroxide solution into the beaker to adjust the pH value to 9-10, putting the beaker into a resistance heating sleeve, raising the temperature in the heating sleeve to 105-110 ℃, and reacting at constant temperature for 130-150 min to prepare reaction slurry; putting the reaction slurry into a glass dish, dropwise adding an acetic acid solution with the mass fraction of 5-10% into the glass dish to adjust the pH value to 6.2-6.5 to prepare a reaction mixture, putting the reaction mixture and cellulase into an enzymolysis tank according to the mass ratio of 100:1, sealing the enzymolysis tank, placing the enzymolysis tank in a greenhouse with the indoor temperature of 30-35 ℃, and standing at constant temperature for 20-24 hours to prepare an enzymolysis reactant; putting the enzymolysis reactant and a standby heat treatment reactant into a reaction kettle according to the mass ratio of 1:4, soaking the mixture in 20-25% of ethanol solution, stirring the mixture by using a stirrer at the rotating speed of 1100-1200 r/min for 50-60 min to prepare dispersion, adding alkyd resin with the mass of 200-300% of the dispersion into the reaction kettle, uniformly stirring the mixture, sealing the reaction kettle after stirring, filling nitrogen into the reaction kettle, raising the pressure in the reaction kettle to 1.6-1.8 MPa, raising the temperature in the reaction kettle to 150-170 ℃, and reacting at constant temperature and constant pressure for 40-60 min to prepare a modified adhesive; spreading and carding cotton fibers, putting the cotton fibers into a glue spraying drying box, uniformly spraying the modified bonding matter on the surfaces of the cotton fibers, wherein the mass of the sprayed modified bonding matter is 15-20% of the mass of the cotton fibers, putting the cotton fibers into a drying oven with the temperature of 70-80 ℃ for standing for 60-80 min after spraying, putting the cotton fibers into a hot press for hot pressing after standing, and trimming and packaging after hot pressing to obtain the high-flame-retardant heat-insulation type glue spraying cotton.