CN112663377A - Preparation method of natural flexible transparent paper - Google Patents
Preparation method of natural flexible transparent paper Download PDFInfo
- Publication number
- CN112663377A CN112663377A CN202011525781.8A CN202011525781A CN112663377A CN 112663377 A CN112663377 A CN 112663377A CN 202011525781 A CN202011525781 A CN 202011525781A CN 112663377 A CN112663377 A CN 112663377A
- Authority
- CN
- China
- Prior art keywords
- paper
- wood pulp
- silicon
- temperature
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Paper (AREA)
Abstract
The invention relates to the field of chemical industry, in particular to a preparation method of natural flexible transparent paper; according to the preparation method of the natural flexible transparent paper, disclosed by the invention, a nano cellulose suspension is added into dissolved wood pulp to be jointly made into base paper, and then the surface of the dried base paper is subjected to hot pressing to prepare the natural transparent paper, wherein the transparent paper can be used as the natural flexible transparent paper and can be applied to the fields of electronic devices such as organic light-emitting diodes, display screens, solar cells and the like; the natural flexible transparent paper has the advantages of high light transparency, low thermal expansion coefficient, good printing performance, flexibility, crimpability and the like, and the natural flexible transparent paper is made of all natural materials and has the advantages of environmental protection, simple process and low cost.
Description
Technical Field
The invention relates to the field of papermaking, in particular to a preparation method of natural flexible transparent paper.
Background
The flexible transparent paper has been successfully applied in the fields of electronic devices such as flexible organic light emitting diodes, display screens, solar cells and the like due to the advantages of low cost, low fragility, flexibility, crimpability and the like.
CN201610341731.1 discloses a full cellulose transparent paper and a preparation method thereof, wherein paper or plant fiber obtained by a traditional paper making process is used as a network framework, a cellulose homogeneous solution with certain solubility is used as a filling agent and a dissolving medium, the filling agent and the dissolving medium are uniformly coated on the surface of the paper or plant fiber, internal pores are filled and cellulose side chains or part of cellulose is dissolved in a high-efficiency and low-cost mode, and the porosity is reduced; the flatness is improved through a post finishing process, an integrated cellulose composite structure is formed, and then a brand-new low-cost holocellulose transparent paper is prepared, so that large-scale roll-to-roll industrial production is expected to be realized.
CN201510960393.5 discloses a transparent paper and a method for rapidly preparing transparent paper by multi-surface coating method. The method comprises the steps of drying the paper-making base paper until the water content is lower than 2%, coating a cellulose solvent on the base paper under the constant temperature condition, carrying out hot pressing treatment under the conditions that the temperature is 80-120 ℃ and the pressure is 1-10MPa, soaking, washing and hot pressing drying. And taking out a sample, and circularly treating the sample for 1-3 times according to the process to obtain the transparent paper with extremely low porosity and compact structure. When the gram weight is 30-60g/m2, the thickness of the transparent paper is 30-100 μm, the light transmittance is 60-90%, the tensile strength is 20-50MPa, and the tensile rate is 10-30%. The invention adopts paper pulp as raw material, has environment-friendly process, low cost and short production period, only needs 30-120min in the whole process, and can realize industrial production by partially reforming the existing paper machine process equipment. CN201810538221.2 discloses a haze-controllable high-transparency paper and a preparation method thereof, and the preparation method comprises the following steps:
(1) the molecular cellulose and the derivatives thereof are used as fillers to provide high light transmittance of the paper; (2) the micron-sized wood fiber forms a three-dimensional porous fiber interwoven network structure through three procedures of fiber fluffing, paper sheet forming and drying. The paper is taken as a framework, so that excellent light scattering performance of the paper is provided; (3) combining the molecular cellulose and the derivatives thereof in the step (1) with the three-dimensional porous fiber interwoven network in the step (2) according to a certain mass ratio by means of a dipping or coating process, and preparing the haze-controllable high-transparency paper by regulating and controlling the quantification of the fiber interwoven network. The light transmittance of the visible light region is 86-91%, and the haze is 0.5-85% (550 nm wavelength). The haze-controllable high-transparency paper has potential application prospects in the fields of LED illumination, flat panel display and photovoltaic devices.
The transparent flexible paper used in the above inventions and prior patents is a flexible organic polymer (polyester, polyimide, polycarbonate, etc.) transparent paper, but the defects of low processing temperature, high thermal expansion coefficient, poor printability and non-recyclability cause the fundamental reason of slow development of flexible organic synthetic polymer paper.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of natural flexible transparent paper.
The paper is produced mainly by three-dimensional interweaving bodies which are composed of plant fibers as main components. When the light beam strikes the sheet, the light is reflected, transmitted, and scattered. Thus, the main factors affecting the transparency of paper include: the method comprises the following steps of (1) preparing a sizing agent and forming a paper sheet by a mode such as pulp beating degree, a paper sheet calendering mode, stress and the like, (2) preparing the type of the sizing agent used in the paper sheet making, (3) containing a small amount of papermaking chemical agents such as fillers, dyes, transparent agents and the like, (4) modifying the surface state of the paper sheet, (5) treating time of the transparent agent, (6) controlling the temperature of the transparent agent, and the like, wherein the refractive index of the paper sheet is the same as that of air, and the light intensity, the light direction and the light propagation speed of the light in a medium are not changed, so that the paper sheet is considered to be ideal colorless transparent paper, secondly, the light irradiated on the paper sheet is completely absorbed, so that the paper sheet is black opaque paper, and thirdly, when the light is completely scattered, the Bei U is white opaque paper [6 ].
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing the dissolved wood pulp into 0.5 to 5 mass percent dissolved wood pulp, adding 20 to 80 mass percent nano cellulose suspension, stirring and mixing evenly, and adopting paper sheetsThe wood pulp is made into base paper by a handsheet machine, the base paper is dried in a drying oven at the temperature of 100 ℃ and 120 ℃ for 60-120min, and then the silicon-containing ionic liquid transparent agent is dried according to the proportion of 0.1-0.8g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 40-60 ℃ for 60-80 min; and then carrying out hot pressing treatment on the base paper at the temperature of 80-120 ℃ and under the pressure of 0.5-5MPa for 5-30min, washing the base paper in ethanol after the treatment is finished, and then carrying out hot pressing repeatedly for 30-60min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 3-8 parts of dissolved wood pulp into a reaction kettle according to the mass parts, adding 280-360 parts of dimethyl sulfoxide and 0.8-2.6 parts of sodium hydroxide, controlling the temperature to be 40-60 ℃, stirring for 30-80min, then adding 2.2-7.4 parts of sodium chloroacetate, controlling the temperature to be 60-80 ℃, and continuously reacting for 10-20 h; after the reaction is finished, washing wood pulp, then preparing wood pulp with the concentration of 0.2-2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 300-1000bar, and the cycle time is 6-12 times; then high-speed centrifugation is carried out, the centrifugation rotating speed is 8000-10000r/min, the time is 3-8min, and the supernatant fluid is taken to be the nano-cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.003-0.012 parts of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.1-1.2 parts of neopentyl glycol polymethyl ethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to be 40-60 ℃, reacting for 0.5-2h, then adding 5-20 parts of 2-ethylhexyl acrylate, 10-25 parts of methyl silicon (glycol) diacetate and 300 parts of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to be 40-60 ℃, reacting for 0.5-2h, then adding 0.3-1.8 parts of tetrakistriphenylphosphine palladium and 1-3.8 parts of magnesium methacrylate into the reaction kettle, and then controlling the temperature to 80-100 ℃, carrying out reflux reaction for 3-8h, and evaporating the solvent after the reaction is finished to obtain the silicon-containing ionic liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 20-40g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The raw material of the silicon-containing ionic liquid transparent agent is selected from 1-allyl-3-methylimidazole hexafluorophosphate ionic liquid.
The raw material of the silicon-containing ionic liquid transparent agent is selected from 1-allyl-3-methylimidazole hexafluorophosphate, neopentyl glycol polymethyl ethylene oxide diacrylate, acrylic acid-2-ethyl hexyl ester and magnesium methacrylate.
The silicon-containing ionic liquid transparent agent raw material is selected from methyl silicon (glycol) diacetate, and the silicon-hydrogen addition reaction is carried out on the raw material containing double bonds and the raw material containing C ═ C double bonds.
The silicon-containing ionic liquid transparent agent is prepared by carrying out hydrosilylation reaction on 1-allyl-3-methylimidazole hexafluorophosphate, magnesium methacrylate and methyl silicon (glycol) diacetate, and a partial addition reaction formula is shown as a diagram.
The action mechanism of the transparentizing agent is that the added silicon-containing ionic liquid transparentizing agent is fully absorbed by the paper and is permeated into the paper, the air in the paper is discharged, the paper sheet and the transparentizing agent can be well integrated, the optical property is uniform, the light transmission is improved, the scattering and the refraction are avoided, and the transparency of the paper is improved. The silicon-containing ionic liquid transparent agent is easy to be fixed on the surface or inside of paper, is not easy to volatilize, has good processing performance, is not easy to deform, has low price, is easy to impregnate and coat, has strong operability, improves the ignition point of hexafluorophosphate groups, is nontoxic and odorless, is easy to dry after the hydrophobic paper is treated, can improve the processing temperature after hydrosilylation, introduces magnesium oxide units into the high molecular chain segment of the natural flexible transparent paper by adding magnesium methacrylate, and can reduce the thermal expansion coefficient of the natural flexible transparent paper.
According to the preparation method of the natural flexible transparent paper, disclosed by the invention, a nano cellulose suspension is added into dissolved wood pulp to be jointly made into base paper, and then the surface of the dried base paper is subjected to hot pressing to prepare the natural transparent paper, wherein the transparent paper can be used as the natural flexible transparent paper and applied to the fields of electronic devices such as organic light-emitting diodes, display screens, solar cells and the like; the natural flexible transparent paper has the advantages of high light transparency, low thermal expansion coefficient, good printing performance, flexibility, crimpability and the like, and the natural flexible transparent paper is made of all natural materials and has the advantages of environmental protection, simple process and low cost.
Drawings
FIG. 1 is a Fourier infrared spectrum of a sample of the silicon-containing ionic liquid clarifier prepared in example 2.
As can be seen from the above figure, the depth of the groove is 1080cm-1The absorption peak of silicon oxygen exists nearby, and is 1414/1260cm-1An absorption peak of silicon carbon exists nearby, which indicates that methyl silicon (glycol) diacetate participates in the reaction; at 1735cm-1An antisymmetric telescopic absorption peak of carbonyl group having ester group in the vicinity of 2960cm-1An antisymmetric telescopic absorption peak of the carbon hydrogen exists nearby, which indicates that the 2-ethylhexyl acrylate participates in the reaction; at 1651cm-1An absorption peak of carbon-nitrogen double bonds exists nearby, which indicates that 1-allyl-3-methylimidazole hexafluorophosphate participates in the reaction; at 1118cm-1An absorption peak of ether bond exists nearby, which shows that neopentyl glycol polymethyl ethylene oxide diacrylate participates in the reaction; 1959cm-1The weaker silicon-hydrogen bond indicates that the silicon-hydrogen bond is reacted, and the silicon-hydrogen addition reaction of methyl silicon (glycol) diacetate is carried out.
Detailed Description
The invention is further illustrated by the following specific examples:
the transparency of the material was determined by means of a UV spectrophotometer (Lambda 35, Perkin Elmer) at a wavelength of 500 nm. The transparent paper was cut into a size of 10mm × 40mm, and the viscoelasticity of the material at 25 ℃ was analyzed using a dynamic thermomechanical analyzer (DMA 242). The mechanical strength was measured using a tensile compression material tester (Instron5565),
the CTE was measured using a thermomechanical analyzer (TMA) in a nitrogen atmosphere at a heating rate of 10 ℃/min and at a temperature range of 30 to 200 ℃ according to astm e 831. The tension used was 0.1N.
Example 1
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into 0.5 percent dissolved wood pulp, then adding 20 to 80 percent nano cellulose suspension, stirring and mixing uniformly, using a paper hand-machine to make the wood pulp into base paper, drying the prepared base paper in a drying oven at 100 ℃ for 60min, and then drying the silicon-containing ionic liquid transparent agent according to 0.1g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 40 ℃ for 60 min; and then carrying out hot pressing treatment on the base paper at the temperature of 80 ℃ and under the pressure of 0.5MPa for 5min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 30min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 3kg of dissolved wood pulp into a reaction kettle, adding 280kg of dimethyl sulfoxide and 0.8kg of sodium hydroxide, controlling the temperature to be 40 ℃, stirring for 30min, then adding 2.2kg of sodium chloroacetate, controlling the temperature to be 60 ℃, and continuously reacting for 10 h; after the reaction is finished, washing wood pulp, then preparing wood pulp liquid with the concentration of 0.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operating pressure is 300bar, and the cycle times are 6 times; then centrifuging at a high speed of 8000r/min for 3min, and taking the supernatant as the nano-cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.003Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.1Kg of neopentyl glycol polymethyloxirane diacrylate into a reaction kettle, stirring and mixing uniformly, controlling the temperature to be 40 ℃, reacting for 0.5h, then adding 5Kg of 2-ethylhexyl acrylate, 10Kg of methyl silicon (glycol) diacetate and 300Kg of n-butyl alcohol, stirring and mixing uniformly, controlling the temperature to be 40 ℃, reacting for 0.5h, then adding 0.3Kg of tetrakistriphenylphosphine palladium, adding 1Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to be 80 ℃, refluxing and reacting for 3h, and evaporating the solvent after the reaction is finished to obtain the silicon-ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 20g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 131.4MPa, the elastic modulus is 264.5MPa, the light transmittance is 88.6 percent, and the thermal expansion coefficient CETs is 7.7 ppm/K.
Example 2
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into dissolved wood pulp with the concentration of 2.5%, then adding 50% of nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 110 ℃ for 90min, and then drying a silicon-containing ionic liquid transparent agent according to the proportion of 0.5g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 50 ℃ for 70 min; and then carrying out hot pressing treatment on the base paper at the temperature of 100 ℃ and under the pressure of 2.5MPa for 15min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 40min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 5kg of dissolved wood pulp into a reaction kettle, adding 320kg of dimethyl sulfoxide and 1.6kg of sodium hydroxide, controlling the temperature to be 50 ℃, stirring for 50min, then adding 4.2kg of sodium chloroacetate, controlling the temperature to be 70 ℃, and continuously reacting for 15 h; after the reaction is finished, washing wood pulp, then mixing the wood pulp with the wood pulp liquid with the concentration of 1.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 800bar, and the cycle times are 9 times; then centrifuging at 9000r/min for 5min at high speed, and collecting the supernatant to obtain nanometer cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.007Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.45Kg of neopentyl glycol polymethylethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to 47 ℃, reacting for 1.5h, then adding 11Kg of 2-ethylhexyl acrylate, 16Kg of methyl silicon (glycol) diacetate and 350Kg of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to 45 ℃, reacting for 1.5h, then adding 0.7Kg of tetrakistriphenylphosphine palladium and 1.9Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to 95 ℃, refluxing and reacting for 5h, and evaporating the solvent after the reaction is finished to obtain the silicon ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 30g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 132.8MPa, the elastic modulus is 266.1MPa, the light transmittance is 89.2 percent, and the thermal expansion coefficient CETs is 7.6 ppm/K.
Example 3
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into 5% dissolved wood pulp, adding 80% nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 120 ℃ for 120min, and then drying a silicon-containing ionic liquid transparent agent according to the proportion of 0.8g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 60 ℃ for 80 min; and then carrying out hot pressing treatment on the base paper at the temperature of 120 ℃ and under the pressure of 5MPa for 30min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 60min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 8kg of dissolved wood pulp into a reaction kettle, adding 360kg of dimethyl sulfoxide and 2.6kg of sodium hydroxide, controlling the temperature at 60 ℃, stirring for 80min, then adding 7.4kg of sodium chloroacetate, controlling the temperature at 80 ℃, and continuously reacting for 20 h; after the reaction is finished, washing wood pulp, then preparing wood pulp with the concentration of 2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operating pressure is 1000bar, and the cycle times are 12 times; then centrifuging at high speed of 10000r/min for 8min, and taking the supernatant as the nano-cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.012Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 1.2Kg of neopentyl glycol polymethyloxirane diacrylate into a reaction kettle, stirring and mixing uniformly, controlling the temperature to be 60 ℃, reacting for 2 hours, then adding 20Kg of 2-ethylhexyl acrylate, 25Kg of methyl silicon (glycol) diacetate and 400Kg of n-butyl alcohol, stirring and mixing uniformly, controlling the temperature to be 60 ℃, reacting for 2 hours, then adding 1.8Kg of tetrakistriphenylphosphine palladium and 3.8Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to be 100 ℃, refluxing and reacting for 8 hours, and evaporating the solvent after the reaction is finished, thus obtaining the silicon-ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 40g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 132.9MPa, the elastic modulus is 270.1MPa, the light transmittance is 89.9 percent, and the thermal expansion coefficient CETs is 7.4 ppm/K.
Comparative example 1
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into dissolved wood pulp with the concentration of 2.5%, then adding 50% of nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 110 ℃ for 90min, and then drying polyvinyl acetate resin according to the proportion of 0.5g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 50 ℃ for 70 min; and then carrying out hot pressing treatment on the base paper at the temperature of 100 ℃ and under the pressure of 2.5MPa for 15min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 40min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 5kg of dissolved wood pulp into a reaction kettle, adding 320kg of dimethyl sulfoxide and 1.6kg of sodium hydroxide, controlling the temperature to be 50 ℃, stirring for 50min, then adding 4.2kg of sodium chloroacetate, controlling the temperature to be 70 ℃, and continuously reacting for 15 h; after the reaction is finished, washing wood pulp, then mixing the wood pulp with the wood pulp liquid with the concentration of 1.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 800bar, and the cycle times are 9 times; then centrifuging at 9000r/min for 5min at high speed, and collecting the supernatant to obtain nanometer cellulose suspension.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 30g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 122.3MPa, the elastic modulus is 187.1MPa, the light transmittance is 61.2 percent, and the coefficient of thermal expansion CETs is 12.6 ppm/K. .
Comparative example 2
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into dissolved wood pulp with the concentration of 2.5%, then adding 50% of nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 110 ℃ for 90min, and then drying a silicon-containing ionic liquid transparent agent according to the proportion of 0.5g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 50 ℃ for 70 min; and then carrying out hot pressing treatment on the base paper at the temperature of 100 ℃ and under the pressure of 2.5MPa for 15min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 40min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 5kg of dissolved wood pulp into a reaction kettle, adding 320kg of dimethyl sulfoxide and 1.6kg of sodium hydroxide, controlling the temperature to be 50 ℃, stirring for 50min, then adding 4.2kg of sodium chloroacetate, controlling the temperature to be 70 ℃, and continuously reacting for 15 h; after the reaction is finished, washing wood pulp, then mixing the wood pulp with the wood pulp liquid with the concentration of 1.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 800bar, and the cycle times are 9 times; then centrifuging at 9000r/min for 5min at high speed, and collecting the supernatant to obtain nanometer cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.007Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.45Kg of neopentyl glycol polymethylethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to 47 ℃, reacting for 1.5h, then adding 11Kg of 2-ethylhexyl acrylate, 16Kg of methyl silicon (glycol) diacetate and 350Kg of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to 45 ℃, reacting for 1.5h, then adding 0.7Kg of tetrakistriphenylphosphine palladium and 1.9Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to 95 ℃, refluxing and reacting for 5h, and evaporating the solvent after the reaction is finished to obtain the silicon ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 30g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 130.8MPa, the elastic modulus is 218.7MPa, the light transmittance is 82.1 percent, and the coefficient of thermal expansion CETs is 7.6 ppm/K.
Comparative example 3
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into dissolved wood pulp with the concentration of 2.5%, then adding 50% of nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 110 ℃ for 90min, and then drying a silicon-containing ionic liquid transparent agent according to the proportion of 0.5g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 50 ℃ for 70 min; then the base paper is processed by hot pressing treatment,the temperature is 100 ℃, the pressure is 2.5MPa, the time is 15min, after the treatment, the base paper is washed in ethanol, and then hot pressing is repeated for 40min, thus obtaining the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 5kg of dissolved wood pulp into a reaction kettle, adding 320kg of dimethyl sulfoxide and 1.6kg of sodium hydroxide, controlling the temperature to be 50 ℃, stirring for 50min, then adding 4.2kg of sodium chloroacetate, controlling the temperature to be 70 ℃, and continuously reacting for 15 h; after the reaction is finished, washing wood pulp, then mixing the wood pulp with the wood pulp liquid with the concentration of 1.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 800bar, and the cycle times are 9 times; then centrifuging at 9000r/min for 5min at high speed, and collecting the supernatant to obtain nanometer cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.007Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.45Kg of neopentyl glycol polymethylethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to 47 ℃, reacting for 1.5h, then adding 11Kg of 2-ethylhexyl acrylate, 16Kg of methyl silicon (glycol) diacetate and 350Kg of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to 45 ℃, reacting for 1.5h, then adding 0.7Kg of tetrakistriphenylphosphine palladium and 1.9Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to 95 ℃, refluxing and reacting for 5h, and evaporating the solvent after the reaction is finished to obtain the silicon ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 30g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 130.2MPa, the elastic modulus is 228.6MPa, the light transmittance is 80.3 percent, and the thermal expansion coefficient CETs is 7.6 ppm/K.
Comparative example 4
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into dissolved wood pulp with the concentration of 2.5%, then adding 50% of nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 110 ℃ for 90min, and then drying a silicon-containing ionic liquid transparent agent according to the proportion of 0.5g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 50 ℃ for 70 min; and then carrying out hot pressing treatment on the base paper at the temperature of 100 ℃ and under the pressure of 2.5MPa for 15min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 40min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 5kg of dissolved wood pulp into a reaction kettle, adding 320kg of dimethyl sulfoxide and 1.6kg of sodium hydroxide, controlling the temperature to be 50 ℃, stirring for 50min, then adding 4.2kg of sodium chloroacetate, controlling the temperature to be 70 ℃, and continuously reacting for 15 h; after the reaction is finished, washing wood pulp, then mixing the wood pulp with the wood pulp liquid with the concentration of 1.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 800bar, and the cycle times are 9 times; then centrifuging at 9000r/min for 5min at high speed, and collecting the supernatant to obtain nanometer cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.007Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.45Kg of neopentyl glycol polymethylethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to 47 ℃, reacting for 1.5h, then adding 11Kg of 2-ethylhexyl acrylate, 16Kg of methyl silicon (glycol) diacetate and 350Kg of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to 45 ℃, reacting for 1.5h, then adding 0.7Kg of tetrakistriphenylphosphine palladium and 1.9Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to 95 ℃, refluxing and reacting for 5h, and evaporating the solvent after the reaction is finished to obtain the silicon ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp.
The base paper has a basis weight of 30g/m2。
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
The tensile strength of the transparent paper material prepared in the experiment is 128.3MPa, the elastic modulus is 242.3MPa, the light transmittance is 83.2 percent, and the coefficient of thermal expansion CETs is 7.6 ppm/K.
Comparative example 5
A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing dissolved wood pulp into dissolved wood pulp with the concentration of 2.5%, then adding 50% of nano cellulose suspension, stirring and mixing uniformly, making the wood pulp into base paper by adopting a paper hand-making machine, drying the prepared base paper in a drying oven at 110 ℃ for 90min, and then drying a silicon-containing ionic liquid transparent agent according to the proportion of 0.5g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 50 ℃ for 70 min; and then carrying out hot pressing treatment on the base paper at the temperature of 100 ℃ and under the pressure of 2.5MPa for 15min, washing the base paper in ethanol after the treatment is finished, and then repeating the hot pressing for 40min to obtain the natural flexible transparent paper.
The preparation method of the nano-cellulose suspension comprises the following steps:
adding 5kg of dissolved wood pulp into a reaction kettle, adding 320kg of dimethyl sulfoxide and 1.6kg of sodium hydroxide, controlling the temperature to be 50 ℃, stirring for 50min, then adding 4.2kg of sodium chloroacetate, controlling the temperature to be 70 ℃, and continuously reacting for 15 h; after the reaction is finished, washing wood pulp, then mixing the wood pulp with the wood pulp liquid with the concentration of 1.2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 800bar, and the cycle times are 9 times; then centrifuging at 9000r/min for 5min at high speed, and collecting the supernatant to obtain nanometer cellulose suspension.
The preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.007Kg of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.45Kg of neopentyl glycol polymethylethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to 47 ℃, reacting for 1.5h, then adding 11Kg of 2-ethylhexyl acrylate, 16Kg of methyl silicon (glycol) diacetate and 350Kg of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to 45 ℃, reacting for 1.5h, then adding 0.7Kg of tetrakistriphenylphosphine palladium and 1.9Kg of magnesium methacrylate into the reaction kettle, controlling the temperature to 95 ℃, refluxing and reacting for 5h, and evaporating the solvent after the reaction is finished to obtain the silicon ion-containing liquid transparent agent.
The dissolving wood pulp is broadleaf wood dissolving wood pulp,
the base paper has a basis weight of 30g/m2，
The surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing,
in the embodiment, magnesium methacrylate is not added, magnesium oxide units cannot be introduced into the natural flexible transparent paper polymer chain segment,
the tensile strength of the transparent paper material prepared in the experiment is 129.5MPa, the elastic modulus is 252.6MPa, the light transmittance is 85.4 percent, and the thermal expansion coefficient CETs is 10.3 ppm/K.
Claims (9)
1. A preparation method of natural flexible transparent paper comprises the following operation steps:
preparing the dissolved wood pulp into 0.5-5% dissolved wood pulp according to the mass part, then adding 20-80% nano cellulose suspension, stirring and mixing uniformly, using a paper hand-making machine to make the wood pulp into base paper, after that, putting the prepared base paper into a drying oven for drying at the temperature of 100 ℃ and 120 ℃ for 60-120min, and then putting a silicon-containing ionic liquid transparent agent according to the mass part of 0.1-0.8g/m2Uniformly coating the raw paper on the surface of the raw paper, standing at 40-60 ℃ for 60-80 min; and then carrying out hot pressing treatment on the base paper at the temperature of 80-120 ℃ and under the pressure of 0.5-5MPa for 5-30min, washing the base paper in ethanol after the treatment is finished, and then carrying out hot pressing repeatedly for 30-60min to obtain the natural flexible transparent paper.
2. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the dissolving wood pulp is broadleaf wood dissolving wood pulp.
3. A natural flexible transparent paper according to claim 1The preparation method is characterized by comprising the following steps: the base paper has a basis weight of 20-40g/m2。
4. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the surface of the base paper is covered with a layer of polytetrafluoroethylene film during hot pressing.
5. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the preparation method of the nano-cellulose suspension comprises the following steps:
adding 3-8 parts of dissolved wood pulp into a reaction kettle according to the mass parts, adding 280-360 parts of dimethyl sulfoxide and 0.8-2.6 parts of sodium hydroxide, controlling the temperature to be 40-60 ℃, stirring for 30-80min, then adding 2.2-7.4 parts of sodium chloroacetate, controlling the temperature to be 60-80 ℃, and continuously reacting for 10-20 h; after the reaction is finished, washing wood pulp, then preparing wood pulp with the concentration of 0.2-2%, and then carrying out high-pressure homogenization by adopting an ultrahigh-pressure nano homogenizer, wherein the operation pressure is 300-1000bar, and the cycle time is 6-12 times; then high-speed centrifugation is carried out, the centrifugation rotating speed is 8000-10000r/min, the time is 3-8min, and the supernatant fluid is taken to be the nano-cellulose suspension.
6. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the raw material of the silicon-containing ionic liquid transparent agent is selected from 1-allyl-3-methylimidazole hexafluorophosphate ionic liquid.
7. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the raw material of the silicon-containing ionic liquid transparent agent is selected from 1-allyl-3-methylimidazole hexafluorophosphate, neopentyl glycol polymethyl ethylene oxide diacrylate, acrylic acid-2-ethyl hexyl ester and magnesium methacrylate.
8. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the silicon-containing ionic liquid transparent agent raw material is selected from methyl silicon (glycol) diacetate, and the silicon-hydrogen addition reaction is carried out on the raw material containing double bonds and the raw material containing C ═ C double bonds.
9. The method of making a natural flexible transparency paper as claimed in claim 1 wherein: the preparation method of the silicon-containing ionic liquid transparent agent comprises the following steps:
adding 0.003-0.012 parts of 1-allyl-3-methylimidazolium hexafluorophosphate and 0.1-1.2 parts of neopentyl glycol polymethyl ethylene oxide diacrylate into a reaction kettle, uniformly stirring and mixing, controlling the temperature to be 40-60 ℃, reacting for 0.5-2h, then adding 5-20 parts of 2-ethylhexyl acrylate, 10-25 parts of methyl silicon (glycol) diacetate and 300 parts of n-butyl alcohol, uniformly stirring and mixing, controlling the temperature to be 40-60 ℃, reacting for 0.5-2h, then adding 0.3-1.8 parts of tetrakistriphenylphosphine palladium and 1-3.8 parts of magnesium methacrylate into the reaction kettle, and then controlling the temperature to 80-100 ℃, carrying out reflux reaction for 3-8h, and evaporating the solvent after the reaction is finished to obtain the silicon-containing ionic liquid transparent agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011525781.8A CN112663377B (en) | 2020-12-22 | 2020-12-22 | Preparation method of natural flexible transparent paper |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011525781.8A CN112663377B (en) | 2020-12-22 | 2020-12-22 | Preparation method of natural flexible transparent paper |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112663377A true CN112663377A (en) | 2021-04-16 |
| CN112663377B CN112663377B (en) | 2021-09-14 |
Family
ID=75407468
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011525781.8A Active CN112663377B (en) | 2020-12-22 | 2020-12-22 | Preparation method of natural flexible transparent paper |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112663377B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804733A (en) * | 2015-05-20 | 2015-07-29 | 江南大学 | Rare-earth strontium aluminate luminous nanorod and preparation method thereof |
| CN105568768A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Transparent paper and method for preparing same by repeatedly coating surface |
| CN105735049A (en) * | 2016-03-31 | 2016-07-06 | 华南理工大学 | Highly-transparent and super-smooth nano-paper and rapid preparation method thereof |
| CN107012737A (en) * | 2017-04-20 | 2017-08-04 | 上海金大塑胶有限公司 | A kind of preparation method of release liners |
| CN109706792A (en) * | 2019-01-04 | 2019-05-03 | 衢州五洲特种纸业股份有限公司 | A kind of transparent release paper and preparation method thereof |
| WO2019158616A1 (en) * | 2018-02-13 | 2019-08-22 | Cmblu Projekt Ag | Novel methods for processing lignocellulosic material |
-
2020
- 2020-12-22 CN CN202011525781.8A patent/CN112663377B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804733A (en) * | 2015-05-20 | 2015-07-29 | 江南大学 | Rare-earth strontium aluminate luminous nanorod and preparation method thereof |
| CN105568768A (en) * | 2015-12-17 | 2016-05-11 | 华南理工大学 | Transparent paper and method for preparing same by repeatedly coating surface |
| CN105735049A (en) * | 2016-03-31 | 2016-07-06 | 华南理工大学 | Highly-transparent and super-smooth nano-paper and rapid preparation method thereof |
| CN107012737A (en) * | 2017-04-20 | 2017-08-04 | 上海金大塑胶有限公司 | A kind of preparation method of release liners |
| WO2019158616A1 (en) * | 2018-02-13 | 2019-08-22 | Cmblu Projekt Ag | Novel methods for processing lignocellulosic material |
| CN109706792A (en) * | 2019-01-04 | 2019-05-03 | 衢州五洲特种纸业股份有限公司 | A kind of transparent release paper and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112663377B (en) | 2021-09-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | A synthesis of a dust suppressant using the cellulose extracted from maize straw | |
| CN106192550B (en) | A kind of cellophane paper and its manufacturing method with regenerated cellulose auxiliary manufacture | |
| CN102276734B (en) | Formaldehyde absorptive reagent capable of improving bonding strength of urea resins as well as preparation method and application thereof | |
| CN113858368B (en) | Preparation method of high-strength flexible wood film | |
| CN103387689A (en) | Method for preparing nanocellulose fiber optical transparent membrane material from peanut hulls | |
| Wang et al. | Preparation and characterization of lignin-acrylamide copolymer as a paper strength additive | |
| CN110952158B (en) | Application of auxiliary agent liquid in preparation of fibroin regenerated cellulose fiber | |
| CN109262783A (en) | A kind of low temperature, atmospheric cooking prepare the method and its application of high-strength transparency cellulose thin-film material | |
| CN113402745B (en) | High-transparency high-strength nanocellulose flexible membrane and preparation method and application thereof | |
| CN110204915A (en) | A kind of preparation method of water proof type nano-cellulose | |
| Zou et al. | Eco-friendly transparent poplar-based composites that are stable and flexible at high temperature | |
| CN112663377B (en) | Preparation method of natural flexible transparent paper | |
| Zheng et al. | Pre-treatment of natural bamboo for use as a high-performance bio-composites via acetic acid ball milling technology | |
| CN108103832A (en) | A kind of photochromic speciality paper and preparation method thereof | |
| CN108841163A (en) | Modified polyurethane resin and preparation method thereof, modified polyurethane artificial leather and application | |
| CN108034205A (en) | A kind of preparation method of peanut shell fibre modification polylactic acid | |
| CN110258141A (en) | A method of improving reactive dye color fixing rate in alcohol organic solvent-aqueous systems | |
| Thang et al. | Fabrication of transparent composites from pinaceae wood packaging residues | |
| CN113787790A (en) | Energy-saving decorative plate and preparation method thereof | |
| CN114230867A (en) | High-wet-strength cellulose composite material and preparation method thereof | |
| CN113957741A (en) | Titanium composite material and application thereof in preparation of base paper | |
| Zhu et al. | Hydrogen Peroxide-oxidized Soybean Polysaccharides as Novel Masking Agents for Zirconium Tanning | |
| CN116285010A (en) | Preparation method of cellulose/seaweed polysaccharide flame-retardant composite material | |
| CN114263065B (en) | Interlayer reinforcing agent for papermaking, raw material composition thereof and preparation method thereof | |
| CN113123158B (en) | Water-resistant transparent paper and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |