CN102031716B - Titanium dioxide air purifying paper doped with rhodium ions and electrostatic spinning preparation method thereof - Google Patents
Titanium dioxide air purifying paper doped with rhodium ions and electrostatic spinning preparation method thereof Download PDFInfo
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- CN102031716B CN102031716B CN 201010519298 CN201010519298A CN102031716B CN 102031716 B CN102031716 B CN 102031716B CN 201010519298 CN201010519298 CN 201010519298 CN 201010519298 A CN201010519298 A CN 201010519298A CN 102031716 B CN102031716 B CN 102031716B
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Abstract
The invention discloses a titanium dioxide air purifying paper doped with rhodium ions and an electrostatic spinning preparation method thereof. The method is as follows: mixing tetraisopropyl titanate, polyvinyl acetate, acetic acid and alcohol, adding rhodium trichloride, stirring and mixing uniformly, and standing; adopting an electrostatic spinning device to carry out electrostatic spinning on the obtained solution at room temperature; then calcining and grinding the collected spinning fiber, thus obtaining titanium dioxide powder doped with rhodium; mixing the titanium dioxide powder doped with rhodium with filler used for pulping and papermaking by an in-pulp adding manner, and preparing the purifying paper by technical process of pulping and papermaking; or dispersing the titanium dioxide powder doped with rhodium and pigments for coating together, adding a coating auxiliary agent to prepare a coating material, coating by utilizing a paper machine coater, and drying to obtain the purifying paper. By adopting an electrostatic spinning method, the nano titanium dioxide doped with rhodium ions is directly prepared; and when the nano titanium dioxide is applied in paper, the paper is ensured to have an air purifying function, and the printing performance of the paper is improved.
Description
Technical field
The present invention relates to air purification paper, particularly relate to titanium dioxide air purification paper and method of electrostatic spinning preparation method thereof that a kind of rhodium ion mixes.
Technical background
Since 21 century; Continuous development along with nanometer technology; Spinning process such as traditional colloid spinning, solvent spinning, melt spinning are because prepared fibre diameter generally all exposes its limitation at micron order gradually; The fibre diameter of electrostatic spinning has the high and big characteristics of surface area of porosity between nanometer and micron, more and more receive extensive concern.
Electrostatic spinning technique is invented in 1934 by Formhals; Common electrostatic spinning apparatus is made up of high voltage source, spinning solution storage facility (band syringe needle) and gathering-device 3 parts; Its principle is to produce high pressure at spray silk syringe needle place, thereby in syringe needle and receiving system, produces electric field.When voltage acquires a certain degree; Polymer in the spinning solution storage facility will under the electric field force effect, overcome viscoelastic power and surface tension ejects the formation jet from syringe needle; Jet is refinement gradually in course of injection; While solvent is wherein evaporated, thereby on gathering-device, forms spinning fibre.
At present, the application of electrostatic spinning technique has been extended to fields such as clothes (nano-fiber for production of non-woven), bio-medical material (artificial nerve, artificial blood vessel, artificial cartilage, artificial skin etc.), ceramic nanofibers, battery diaphragm, sensor from early stage molecular filtration filtering material.Overweight the research of traditional textile fabric aspect for the external research major side of electrostatic spinning, like U.S. Pat 6,110,590 disclose a kind of method of using the network bride spider's thread and mulberry silk to prepare nano non-woven fabric, and fibre diameter is 2～2000 nanometers.
Utilize electrospinning process to obtain the existing report of anti-biotic material; For example Shenglian International Biological Sci. & Tech. Co., Ltd. is to use electrospinning process that Nano Silver is embedded in the polyacrylic nanofiber in the application for a patent for invention of CN 1851087A to form nano silver fiber net, obtained good antibacterial performance at publication number.
Yet it is also comparatively rare to utilize electrospinning process to prepare the report of nano titanium oxide material for air purification.In fact, the phenomenon that usually exists formaldehyde, volatile organic matter pernicious gases such as (benzene, toluene) to exceed standard in indoor (especially newly-decorated room) air.According to statistics, interior decoration after 6 months concentration of formaldehyde still exceed standard usually more than 3 times, fit up after 3 years, the mean concentration of indoor benzene series thing is still outdoor 2～4 times.
Common air purification method has at present: strengthen methods such as circulation of air, charcoal absorption, perfuming technology and negative oxygen ion technology, these methods receive many restrictions such as place, adsorbance and security.And nano titanium oxide uses sunshine as the energy, can decompose the gas that is detrimental to health, and nano titanium oxide itself and no consumption, does not produce secondary pollution.
Summary of the invention
The objective of the invention is to overcome the shortcoming of present existing material for air purification and method, provide both to make paper have air-cleaning function, improve the method for electrostatic spinning preparation method of the titanium dioxide air purification paper that the rhodium ion of paper printing characteristic mixes again.
Another purpose of the present invention is to provide the titanium dioxide air purification paper according to the rhodium ion doping of method for preparing.
The object of the invention is realized through following technical scheme:
The method of electrostatic spinning preparation method of the titanium dioxide air purification paper that a kind of rhodium ion mixes may further comprise the steps:
(1) solution preparation: with isopropyl titanate, polyvinyl acetate, acetic acid and ethanol with mass ratio 0.9～1.1: 0.9～1.1: 0.9～1.1: after 2.9～3.1 mixed; Add rhodium chloride; Control rhodium element and titanium elements mass ratio are 0.1～1: 100; Mix, left standstill 1.5～2 hours; Said polyvinyl acetate solid content is 50～60%;
(2) electrostatic spinning: adopt electrostatic spinning apparatus at room temperature to carry out electrostatic spinning the solution of step (1) gained;
(3) spinning fibre of collecting is put into calcining furnace; Be warming up to 190～200 ℃ of insulations 3.5～4 hours with 10～15K/min heating rate; Be warming up to 560～580 ℃ of insulation 40～50min with 10～15K/min heating rate again, the spinning fibre after the calcining cooled off at room temperature to be ground to particle diameter be 200～400nm;
The titania powder that (4) will mix with respect to the rhodium of oven dry stock quality 0.5～2.0% mixes with the filler that pulping and paper-making uses through addition manner in starching, and makes the titanium dioxide air purification paper through the papermaking flow process; Or the titania powder that will mix with respect to the said rhodium of pigment mass 4～12% disperses with pigment with coating; Add coating additive again and be made into coating; Be coated with the back oven dry at paper machine coating machine and obtain the titanium dioxide air purification paper, the coating coating weight is 30 ± 2g/m
2
For further realizing the object of the invention, mixing of said step (1) is that 500～1000rpm condition lower magnetic force stirred 3.5～4 hours at rotating speed preferably.
Said electrostatic spinning is to be 50～55% in control relative humidity, syringe needle to collecting board distance 18～20cm, and spinning voltage 16～18kV carries out under syringe flow 60～80 μ L/min conditions.
Said syringe volume is preferably 10 milliliters, and the syringe needle diameter is preferably 0.5mm.
Described isopropyl titanate purity >=98%; The concentration of acetic acid >=99.5%; The purity of ethanol >=99%; The purity of rhodium chloride >=99%.
In mass fraction, the composition of coating is preferably in the said step (4): 4～12% parts of nano titanium oxides, 67～68 parts of china clay; 32～33 parts in 90 grades of calcium carbonate; 13～14 parts of carboxylic styrene butadiene latexs, 1 part of stearate soap lubricant, 0.9～1 part of polyamide polyureas water repellent agent; 0.5～0.6 part of carboxymethyl cellulose, 0.1～0.2 part of 0.1 part of organosilicon foam inhibitor and polyether antifoam agent.
Need to prove that china clay, 90 grades of calcium carbonate, carboxylic styrene butadiene latex, stearate soap lubricant, polyamide polyureas water repellent agent, carboxymethyl cellulose, organosilicon foam inhibitor and polyether antifoam agents all are this area coating raw materials commonly used.
By the titanium dioxide air purification paper that the rhodium ion of method for preparing mixes, cubage by mass percentage, TiO in the paper
2Content is 0.4～1.6%.
With respect to prior art, the present invention has following advantage:
Conventional method of ventilation is best to the clean-up effect of room air; But receive the restriction of place, safety; Charcoal absorption exists adsorbance to be prone to saturated problem; And to the just absorption and really not removing of airborne pollutant, the perfuming technology has also just been covered up the taste of pollutant in the air, and the negative oxygen ion The Application of Technology is then owing to it also clearly is not restricted the health Influence on security.Therefore, the nano titanium dioxide photocatalysis technology is owing to good air purification effect receives extensive concern, and sol-gel process is the method for using always for preparing nano titanium oxide; Complex process; Consuming time longer, and the difficult control of hydrolysis of alkoxide, the present invention adopts the method for electrostatic spinning directly to prepare the nano titanium oxide that rhodium ion mixes; Thereby improve its visible light respective performances, and apply it in the paper and go.Compare with traditional sol-gel process, method of electrostatic spinning can directly make nano level titania fiber, after calcining, contains hole small, no fixed orientation; Has bigger specific area simultaneously; Reactivity is higher, makes its bactericidal property obviously improve, and adopts interior interpolation of slurry or coating process to combine with traditional paper industry process flow process; Need not to carry out big change, be convenient to carry out the production of air purification paper.
The specific embodiment
Below in conjunction with embodiment the present invention is further described, but the scope that the present invention requires to protect is not limited to the scope that embodiment expresses.The % that does not specify in the embodiment of the invention is meant mass percent.
Embodiment 1: with isopropyl titanate (purity 98%), polyvinyl acetate (solid content 55%), acetic acid (purity 99.6%), ethanol (purity 99%) with mass ratio 0.9: 1: 1.1: 2.9 mixed; Carry out magnetic agitation 3.5 hours (rotating speed 500rpm) after adding rhodium chloride (rhodium element and titanium elements mass ratio=1: 100), left standstill 2 hours.Adopt electrostatic spinning apparatus (10 milliliters of syringe volumes, syringe needle diameter 0.5mm) at room temperature to carry out electrostatic spinning, control relative humidity 50%, syringe needle to collecting board is apart from 18cm, spinning voltage 16kV, flow 60 μ L/min.Adopt Muffle furnace to calcine the spinning fibre of collecting; Muffle furnace heating rate 15K/min is warming up to 200 ℃ of insulations 4 hours, is warming up to 580 ℃ with the 15K/min heating rate again; Insulation 40min; Spinning fibre after the calcining is at room temperature cooled off grinding, obtain nano titanium dioxide powder, particle diameter is 250～300nm.To mix with 325 order talcum powder with respect to the nano titanium dioxide powder of oven dry stock quality 0.5%, 1%, 1.5%, 2% respectively with respect to oven dry stock quality 10%; Add to and join paper supply machine use in the stock tank; The stock quality proportioning is 20% needlebush and 80% leaf wood; Mix 30 ° of SR of beating degree, the Substance of manufacturing paper with pulp is 40g/m
2, TiO in the nano titanium oxide air purification paper that makes
2Mass content is respectively 0.4%, 0.8%, 1.2% and 1.6%.
Embodiment 2: with isopropyl titanate (purity 99%), polyvinyl acetate (solid content 60%), acetic acid (purity 99.5%), ethanol (purity 99%) with mass ratio 1: 0.9: 0.9: 3.1 mixed; The adding rhodium chloride (rhodium element and titanium elements mass ratio=0.1: 100) carry out magnetic agitation 4 hours (rotating speed 600rpm), left standstill 2 hours.Adopt electrostatic spinning apparatus (10 milliliters of syringe volumes, syringe needle diameter 0.5mm) at room temperature to carry out electrostatic spinning, control relative humidity 50%, syringe needle to collecting board is apart from 19cm, spinning voltage 17kV, flow 70 μ L/min.Adopt Muffle furnace to calcine the spinning fibre of collecting; Heating rate 10K/min is warming up to 190 ℃ of insulations 3.5 hours; Be warming up to 580 ℃ of insulation 40min with the 15K/min heating rate again, sample at room temperature cooled off grinding obtain nano titanium dioxide powder, particle diameter is 200～250mm.To be that 325 order talcum powder of 10% (with respect to oven dry stock) mix with respect to the nano titanium dioxide powder of oven dry stock 0.8% and mass percent; Add to and join paper supply machine use in the stock tank; Wet end furnish is 30% needlebush and 70% leaf wood; Mix 40 ° of SR of beating degree, the Substance of manufacturing paper with pulp is 80g/m
2, become TiO in the paper
2Mass content is 0.6%.
Embodiment 3: with isopropyl titanate (purity 99%), polyvinyl acetate (solid content 55%), acetic acid (purity 99.5%), ethanol (purity 99%) with mass ratio 0.9: 1: 0.9: 3.1 mixed; The adding rhodium chloride (rhodium element and titanium elements mass ratio=0.5: 100) carry out magnetic agitation 4 hours (rotating speed 800rpm), left standstill 1.5 hours.Adopt electrostatic spinning apparatus (10 milliliters of syringe volumes, syringe needle diameter 0.5mm) at room temperature to carry out electrostatic spinning, control relative humidity 52%, syringe needle to collecting board is apart from 19cm, spinning voltage 17kV, flow 60 μ L/min.Adopt Muffle furnace to calcine the spinning fibre of collecting; Heating rate 10K/min is warming up to 190 ℃ of insulations 4 hours; Be warming up to 570 ℃ of insulation 40min with the 15K/min heating rate again, sample at room temperature cooled off grinding obtain titania powder, particle diameter is 350～400nm.To be that 325 order talcum powder of 8% (with respect to oven dry stock) mix with respect to the nano titanium dioxide powder of oven dry stock 0.8% and mass percent; Add to and join paper supply machine use in the stock tank; Wet end furnish is 40% needlebush and 70% leaf wood; Mix 48 ° of SR of beating degree, the Substance of manufacturing paper with pulp is 90g/m
2, become TiO in the paper
2Mass content is 0.64%.
Embodiment 4: with isopropyl titanate (purity 99%), polyvinyl acetate (solid content 60%), acetic acid (purity 99.5%), ethanol (purity 99.5%) with mass ratio 1: 1: 0.9: 2.9 mixed; The adding rhodium chloride (rhodium element and titanium elements mass ratio=0.3: 100) carry out magnetic agitation 4 hours (rotating speed 700rpm), left standstill 2 hours.Adopt electrostatic spinning apparatus (10 milliliters of syringe volumes, syringe needle diameter 0.5mm) at room temperature to carry out electrostatic spinning, control relative humidity 52%, syringe needle to collecting board is apart from 20cm, spinning voltage 16kV, flow 75 μ L/min.Adopt Muffle furnace to calcine the spinning fibre of collecting; Heating rate 15K/min is warming up to 200 ℃ of insulations 4 hours; Be warming up to 580 ℃ of insulation 50min with the 15K/min heating rate again, sample at room temperature cooled off grinding obtain nano titanium dioxide powder, particle diameter is 350～400nm.With mass percent is that nano titanium dioxide powder and the coating pigment (68 parts of china clay, 90 grades calcium carbonate 32 parts) of 10% (with respect to pigment) mixes, and adds coating additive again and processes coating and be coated with the back oven dry and obtain air purification paper.In mass fraction, coating consists of: 10 parts of nano titanium dioxide powders, 68 parts of china clay; 32 parts in 90 grades of calcium carbonate, 13 parts of carboxylic styrene butadiene latexs, 1 part of stearate soap lubricant; 0.9 part of polyamide polyureas water repellent agent; 0.6 part of carboxymethyl cellulose, 0.1 part of organosilicon foam inhibitor, 0.2 part of polyether antifoam agent.Coating solid content 61～62%, and viscosity 1000～1200mPas (No. 3 rotors, 60rpm), pH9～9.5.The Substance of manufacturing paper with pulp is 250g/m
2, coating weight 30 ± 2g/m
2, become TiO in the paper
2Mass content is 1.2%.
Embodiment 5: with isopropyl titanate (99%), polyvinyl acetate (solid content 50%), acetic acid (purity 99.5%), ethanol (purity 99%) with mass ratio 0.9: 0.9: 0.9: 3 mixed; The adding rhodium chloride (rhodium element and titanium elements mass ratio=0.7: 100) carry out magnetic agitation 4 hours (rotating speed 1000rpm), left standstill 1.5 hours.Adopt electrostatic spinning apparatus (10 milliliters of syringe volumes, syringe needle diameter 0.5mm) at room temperature to carry out electrostatic spinning, control relative humidity 53%, syringe needle to collecting board is apart from 19cm, spinning voltage 16kV, flow 65 μ L/min.Adopt Muffle furnace to calcine the spinning fibre of collecting; Heating rate 15K/min is warming up to 200 ℃ of insulations 4 hours; Be warming up to 580 ℃ of insulation 40min with the 15K/min heating rate again, sample at room temperature cooled off grinding obtain nano titanium dioxide powder, particle diameter is 300～350nm.With mass percent is that nano titanium dioxide powder and the coating pigment (67 parts of china clay, 90 grades calcium carbonate 33 parts) of 4%, 8%, 12% (with respect to pigment) mixes, and adds coating additive again and processes coating and be coated with the back oven dry and obtain air purification paper.In mass fraction, coating consists of: nano titanium oxide is respectively 4 parts, 8 parts, 12 parts, 67 parts of china clay; 33 parts in 90 grades of calcium carbonate, 14 parts of carboxylic styrene butadiene latexs, 1 part of stearate soap lubricant; 1 part of polyamide polyureas water repellent agent; 0.5 part of carboxymethyl cellulose, 0.1 part of organosilicon foam inhibitor, 0.1 part of polyether antifoam agent.Coating solid content 60～62%, and viscosity 1100～1200mPas (No. 3 rotors, 60r/min), pH9～9.5.The Substance of manufacturing paper with pulp is 300g/m
2, coating weight 30+2g/m
2, become TiO in the paper
2Mass content is respectively 0.4%, 0.8% and 1.2%.
The titanium dioxide air purification paper that the rhodium ion that uses the present invention's preparation is mixed has carried out the detection to trace formaldehyde purifying property and paper performance in the air; The pattern experimental result of table 1 for making according to embodiment 1, the pattern experimental result of table 2 for making according to embodiment 5.Embodiment 2,3 results are similar with embodiment 1; Embodiment 4 is similar with embodiment 5 results.
Table 1
| Content of titanium dioxide (%) | 0 | 0.4 | 0.8 | 1.2 | 1.6 |
| Substance (g/m 2) | 40.2 | 39.7 | 40.4 | 39.5 | 39.4 |
| Become paper whiteness (%ISO) | 72.3 | 73.4 | 73.9 | 74.4 | 74.8 |
| Degradation Formaldehyde rate (%) | 0 | 45.8 | 66.3 | 88.2 | 90.3 |
Can find out that from table 1 the purifying formaldehyde effect of air purification paper increases along with adding the rising of content of titanium dioxide in the slurry, and become the whiteness of paper to increase, improve the texture of paper performance.
Table 2
| Content of titanium dioxide (%) | 0 | 0.4 | 0.8 | 1.2 |
| Substance (g/m 2) | 301.2 | 300.8 | 302.1 | 299.6 |
| Become paper whiteness (%ISO) | 85.5 | 85.9 | 86.1 | 86.9 |
| Smoothness (s) | 120 | 122 | 123 | 125 |
| Degradation Formaldehyde rate (%) | 0 | 51.2 | 76.3 | 92.1 |
Can find out from table 2,, become the Degradation Formaldehyde rate of paper to improve, and become paper whiteness and smoothness also to rise to some extent, can improve printing effect along with the increase of content of titanium dioxide in the coating.
This shows; The air purification paper of the present invention's preparation has good air purification effect; Other character of titanium dioxide powder foot couple paper that the interpolation method of electrostatic spinning prepares the rhodium ion doping do not have influence basically; But also can improve printing performance, applicable to paper kinds such as paper for daily use, cultural paper, package papers.
Claims (7)
1. the method for electrostatic spinning preparation method of the titanium dioxide air purification paper that mixes of a rhodium ion is characterized in that may further comprise the steps:
(1) solution preparation: with isopropyl titanate, polyvinyl acetate, acetic acid and ethanol with mass ratio 0.9～1.1: 0.9～1.1: 0.9～1.1: after 2.9～3.1 mixed; Add rhodium chloride; Control rhodium element and titanium elements mass ratio are 0.1～1: 100; Mix, left standstill 1.5～2 hours; Said polyvinyl acetate solid content is 50～60%;
(2) electrostatic spinning: adopt electrostatic spinning apparatus at room temperature to carry out electrostatic spinning the solution of step (1) gained;
(3) spinning fibre of collecting is put into calcining furnace; Be warming up to 190～200 ℃ of insulations 3.5～4 hours with 10～15K/min heating rate; Be warming up to 560～580 ℃ of insulation 40～50min with 10～15K/min heating rate again, the spinning fibre after the calcining cooled off at room temperature to be ground to particle diameter be 200～400nm;
The titania powder that (4) will mix with respect to the rhodium of oven dry stock quality 0.5～2.0% mixes with the filler that pulping and paper-making uses through addition manner in starching, and makes the titanium dioxide air purification paper through the papermaking flow process; Or the titania powder that will mix with respect to the said rhodium of pigment mass 4～12% disperses with pigment with coating; Add coating additive again and be made into coating; Be coated with the back oven dry at paper machine coating machine and obtain the titanium dioxide air purification paper, the coating coating weight is 30 ± 2g/m
2
2. the method for electrostatic spinning preparation method of the titanium dioxide air purification paper that rhodium ion according to claim 1 mixes is characterized in that: mixing of said step (1) is to be that 500～1000rpm condition lower magnetic force stirred 3.5～4 hours at rotating speed.
3. the method for electrostatic spinning preparation method of the titanium dioxide air purification paper that rhodium ion according to claim 1 mixes; It is characterized in that: said electrostatic spinning be control relative humidity be 50～55%; Syringe needle to collecting board distance 18～20cm; Spinning voltage 16～18kV carries out under syringe flow 60～80 μ L/min conditions.
4. the method for electrostatic spinning preparation method of the titanium dioxide air purification paper that rhodium ion according to claim 3 mixes, it is characterized in that: said syringe volume is 10 milliliters, the syringe needle diameter is 0.5mm.
5. the method for electrostatic spinning preparation method of the titanium dioxide air purification paper that rhodium ion according to claim 1 mixes is characterized in that: described isopropyl titanate purity >=98%; The concentration of acetic acid >=99.5%; The purity of ethanol >=99%; The purity of rhodium chloride >=99%.
6. the titanium dioxide air purification paper that rhodium ion mixes is characterized in that by the said method preparation of claim 1.
7. the titanium dioxide air purification paper that rhodium ion according to claim 6 mixes is characterized in that cubage by mass percentage, TiO in the paper
2Content is 0.4～1.6%.
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