CN107572887A - A kind of preparation method of antibacterial artificial quartz sheet material - Google Patents
A kind of preparation method of antibacterial artificial quartz sheet material Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of antibacterial artificial quartz sheet material, comprise the following steps：（1）Each raw material is weighed by proportioning, and it is separated；The parts by weight of wherein each raw material are as follows：88 92 parts of aggregate, 8 12 parts of resin, 0.6 1 parts of curing agent, 0.8 1 parts of coupling agent, 0.1 2 parts of colorant, 13 parts of antiseptic, 12 parts of natural lignin；（2）Antiseptic is added in resin, is stirred under vacuum mixing；Then colorant, coupling agent, aggregate, natural lignin are added, is stirred under vacuum mixing；Curing agent is eventually adding, mixing is stirred under vacuum, obtains compound；（3）Compound is evenly laid out in template；（4）Shutter vibration is compressing；（5）Solidification for the first time is carried out successively and second solidifies.The present invention is effectively improved the mechanical performances such as hardness, the toughness of synthetic quartz slabstone by the optimization to composition of raw materials, improvement, the mutual cooperation of different material, and antimicrbial power is strong, and antibacterial action is lasting, improves the combination property of synthetic quartz slabstone.
Description
Technical field
The present invention relates to building decoration technology field, more particularly to a kind of preparation side of antibacterial artificial quartz sheet material
Method.
Background technology
Artificial quartz in lump（Or Buddha's warrior attendant/hard rock）Cradle is cried when entering Chinese within 2005 and matches sharp stone in Spain,
After artificial quartz in lump is approved by increasing consumer, China in 2006 starts someone and researches and develops artificial quartz in lump, 2007
Year successively has many producers to be proposed domestic artificial quartz in lump.Artificial quartz in lump is as new Artificial construction material, moistureproof, anti-
Acid, spelling property etc. have the advantages of lithotome is incomparable.In natural stone resource increasingly exhausted today, artificial stone
Diamond stone is its best substitute.Meanwhile artificial quartz in lump can make raw material using discarded glass, thus while environmental protection
Resource reutilization is realized, these advantages allow artificial quartz in lump to turn into the upstart of architectural decoration, therefore, are widely used in
The public buildings such as hotel, dining room, bank, hospital, exhibition, laboratory and kitchen countertop, commode, kitchen and bath's metope, dining table, tea
The house decoration such as several, windowsill, door pocket field.
However, artificial quartz in lump of the prior art also has the shortcomings that its is intrinsic, for example, artificial quartz in lump when in use its
The effect of surface can be contaminated by bacterial unavoidably, but common artificial quartz in lump does not suppress or killed to bacterium.
The content of the invention
The defects of in order to make up prior art, the present invention provide a kind of preparation method of antibacterial artificial quartz sheet material.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of preparation method of antibacterial artificial quartz sheet material, comprises the following steps：
（1）Each raw material is weighed by proportioning, and it is separated；The parts by weight of wherein each raw material are as follows：Aggregate 88-92 parts, tree
Fat 8-12 parts, curing agent 0.6-1 parts, coupling agent 0.8-1 parts, colorant 0.1-2 parts, antiseptic 1-3 parts, natural lignin 1-2
Part；The aggregate is made up of granular filler and powder filler, and the percentage by weight of granular filler is 20-30%, the weight of powder filler
Measuring percentage is：70-80%；The granular filler is the glass particle and quartz sand particle that particle size is 5-60 mesh, glass
The ratio of weight and number of grain and quartz sand particle is 2:3；The powder filler be silica flour that particle size is 160-1200 mesh and
Heavy carbonic calcium powder, its ratio of weight and number are 1:2；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then add colorant, coupling agent, aggregate,
Natural lignin, it is stirred under vacuum 6~8min of mixing；Curing agent is eventually adding, 6~8min of mixing is stirred under vacuum, obtains compound；
（3）Compound is evenly laid out in template；
（4）Template is sent into vacuum vibration formation pressing machine and vibrates compressing, the vacuum in the vacuum vibration formation pressing machine
Degree control be -0.1~-0.08MPa, and the control of vacuum vibration formation pressing machine working frequency is 50Hz, and the static pressure on pressure head controls
For 30~50kg, 180~300s is suppressed；
（5）After vibration is compressing, solidification for the first time being carried out successively and is solidified for the second time, the temperature of the first time solidification is
60~80 DEG C, 15~20 minutes time；Second of 100 ± 2 DEG C of solidification temperature, hardening time are 10~20 minutes；
（6）After the completion of solidification, the room temperature completely rear sheet material thicknessing machine that enters to be cooled is fixed thick, then enters by water mill polissoir
Row polishing.
Material is successively added in the present invention and carries out vacuum stirring mixing, it is therefore intended that is eliminated that may be present in compound
Bubble, the finished product material that so manufactures is finer and closely woven, intensity is higher, surface is more bright and clean attractive in appearance.
Solidified at twice in the present invention, in order to ensure that curing reaction is steadily carried out, solidification safety, avoid anti-
Should be too fierce, produce stomata and waste material.
In the present invention, described natural lignin is the powdered of granularity≤2cm.The natural lignin refers to from containing wood
In the plant of quality, to separate the lignin obtained the methods of physical crushing, solvent extraction, biodegradation, chemical breakdown.This hair
Lignin is with the addition of in bright, on the one hand, lignin is network-like high polymer, after it and resin, aggregate are compound, forms crosslinking
Network structure, improve the performance of sheet material；On the other hand, lignin contains many phenolic hydroxyl groups, is natural antiseptic, has
Bioactivity, antibacterial effect can be improved.
Further, the one kind of the resin in epoxy resin, phenolic resin, acrylic resin, polyurethane resin.
Further, the coupling agent is γ-methacryloxypropyl trimethoxy silane, γ-(2,3- the third oxygen of epoxy)
Propyl trimethoxy silicane, N- β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N- (β-aminoethyl)-γ-ammonia third
Ethyl triethoxy silicane alkane, N- β (aminoethyl)-γ-aminopropyltrimethoxysilane, anilinomethyl triethoxysilane, γ-ammonia
Propyl-triethoxysilicane, VTES, vinyltrimethoxy silane and γ-chloropropyl triethoxy silicon
One kind in alkane.
Further, the curing agent is made up of the composition of following percentage by weight：AMBN 16%, peroxidating
Benzoyl 21%, peroxidating (2 ethyl hexanoic acid) tert-butyl ester 63%.
Curing agent huge number, the present inventor are screened to substantial amounts of curing agent, optimized, and determine to be adapted to so as to screen
The curing agent added in artificial quartz in lump is made up of the composition of following percentage by weight：AMBN 16%, benzoyl peroxide
Formyl 21%, peroxidating (2 ethyl hexanoic acid) tert-butyl ester 63%.Inventor has found that peroxidating (2- ethyls are used merely
Caproic acid) for the tert-butyl ester as curing agent, the artificial quartz in lump internal stress of preparation is big, easy to crack, and add benzoyl peroxide can be with
Above mentioned problem is avoided, but artificial quartz in lump can be caused to shrink the problem of big, hardness is inadequate simultaneously.And the present invention is different using azo two
Valeronitrile, benzoyl peroxide and peroxidating (2 ethyl hexanoic acid) tert-butyl ester compounding are used as curing agent, and rationally control its dosage to match somebody with somebody
Than each component cooperates, synergy so that the internal stress of the artificial quartz in lump of preparation is small, and performance can reach maximum table
It is existing, initiation temperature and energy consumption are reduced while the curing degree and solidify afterwards performance of artificial quartz stone plate is improved, is improved solid
The curing efficiency of agent, the curing efficiency of curing agent of the invention are 3~4 times of traditional curing agent.
Further, the antiseptic is using the homogeneous mixture of modified zeolite and crude tourmaline as complex carrier,
The nano titanium oxide of selenium nitrogen tungsten codope is loaded on complex carrier, in described complex carrier, modified zeolite and it is natural electrically
The weight ratio of stone is（2-3）∶1.
Further, the preparation method of the antiseptic is：
（1）Isopropyl titanate, isopropanol and triethanolamine are mixed and stirred for 1.5-2 hours and obtain the first solution, wherein metatitanic acid
Isopropyl ester, isopropanol, the volume ratio of triethanolamine are 1:（5-6）：0.8；
（2）Selenium powder and oxalic acid are added in deionized water, are uniformly mixing to obtain the second solution, wherein, mole of selenium powder and oxalic acid
Than for 1:3, the mol ratio of selenium powder and isopropyl titanate is 1:15；
（3）Urea and citric acid are added in deionized water, are uniformly mixing to obtain the 3rd solution, wherein, urea and citric acid
Mol ratio is 1:1.5, the mol ratio of urea and isopropyl titanate is 1:20；
（4）Ammonium tungstate and pyrolkigneous liquid are added in deionized water, obtain the 4th solution, wherein, mole of ammonium tungstate and pyrolkigneous liquid
Than for 1:2, the mol ratio of ammonium tungstate and isopropyl titanate is 1:30；
（5）Second solution, the 3rd solution and the 4th solution are mixed into the 4th solution, wherein the volume of the 4th solution is 30ml；
（6）By modified zeolite and crude tourmaline by weight（2-3）：1 mixing, then ultra-fine grinding to average grain diameter are less than 5.0 μ
M, obtain complex carrier；
（7）In the presence of ultrasonic wave, the 4th solution is added dropwise in above-mentioned first solution, adds above-mentioned complex carrier,
Continue stir 1-3 hours obtain colloidal sol；
（8）It is put into after obtained colloidal sol is placed into ageing 2~3 days in Muffle furnace, 190 is warming up to 5~10 DEG C/minute of programming rates
~200 DEG C are incubated 3.5~4 hours, then are warming up to 550~580 DEG C of 40~50min of insulation with 12~15 DEG C/heating rate, with stove
It is cooled to and takes out cooling to be at room temperature ground to particle diameter be 200~400nm.
Further, the preparation method of the modified zeolite is：Stellerite ore is eluriated, crushing and processing to 560-
580 mesh；It is acidified using 1g epidesmine 0.1M hydrochloric acid 40ml as ratio, by the epidesmine and 15% sodium chloride after acidifying
Stirring reaction 3 hours under insulation, place 2 hours, washed to neutrality at room temperature, modified zeolite is obtained after drying.Using above-mentioned side
The modified zeolite that method obtains can partial removal zeolitic frameworks aluminium and the deposit that removes in duct form continuous empty passage,
Increase Zeolite and specific surface area, increase substantially its absorption property and heat endurance.Antiseptic is used as using modified zeolite
Carrier, the titanium dioxide of selenium nitrogen tungsten codope is efficiently distributed.
Titanium dioxide has two kinds of crystal formations of anatase titanium dioxide and rutile-type.With chemical property is stable, nontoxic, non-stimulated, Qiang Ping
The features such as covering ultraviolet.Titanium dioxide can not only influence bacterial reproduction power, moreover it is possible to destroy the membrane structure of bacterium, reach thorough
The purpose of bacterium for degrading.Nano titanium oxide belongs to non-dissolving type material, while degradable organic pollutant and killing bacterium, from
Body does not decompose, not dissolution, and photocatalysis is lasting, and with lasting sterilization, degradation of contaminant effect.The present invention uses selenium nitrogen
The nano titanium oxide of tungsten codope, compared with undoped nano titanium oxide, due to selenium, nitrogen, tungsten synergy, make
The band gap of titanium dioxide becomes narrower, therefore the response enhancing to visible ray, and suppresses the compound of electron-hole, simultaneously
Lattice defect is formd, advantageously forms more Ti3+Oxidation center so that its bactericidal property significantly improves.
Natural antibacterial agent pyrolkigneous liquid is with the addition of in the present invention, pyrolkigneous liquid can be attracted in the empty passage of modified zeolite,
More permanent antibacterial activity can be provided, there is the advantages of safety, green.
The nano titanium dioxide powder of selenium nitrogen tungsten codope is asked in application in the presence of what easy reunion, hardly possible were disperseed in the present invention
Topic, and drawbacks described above can be overcome by being carried on above-mentioned complex carrier.
Titanium dioxide is under light action in the present invention, and being activated produces the hole of electronegative electronics and positively charged and be
Row reaction, forms hole-electron pair, hydroxyl and the oxygen molecule capture that these both hole and electrons are adsorbed by titanium dioxide surface, generation
Hydroxyl radical free radical and superoxide anion radical, newly-generated free radical contact bacterium, they with bacterial cell in group
Reacted into composition, kill bacterium and play a part of antibacterial, and titanium dioxide in itself will not dissolution and decomposition, play and persistently kill
The effect of bacterium.But above-mentioned reaction needs a certain amount of hydrone, and the modified zeolite and crude tourmaline in the present invention can be with
Sufficient hydrone is provided, promotes the sterilization of titanium dioxide.
The nano titanium oxide of selenium nitrogen tungsten codope can preferably absorb the energy in sunshine in the present invention, there is provided give
Tourmaline, the anion releasability of tourmaline is improved, it is that have to the tourmaline in complex carrier in terms of antibacterial efficacy
The component of humidification, both have synergistic function, and antimicrbial power is strong, and antibacterial action is lasting.
The present invention has the advantages that：
The present invention is effectively improved artificial quartz in lump by the optimization to composition of raw materials, improvement, the mutual cooperation of different material
The mechanical performances such as the hardness of plate, toughness, and antimicrbial power is strong, antibacterial action is lasting, improves the combination property of synthetic quartz slabstone.
Embodiment
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Embodiment 1
A kind of antibacterial artificial quartz sheet material, it is made up of the raw material of following parts by weight：90 parts of aggregate, 10 parts of resin, solidification
0.8 part of agent, 0.9 part of coupling agent, 1 part of colorant, 2 parts of antiseptic, 1.5 parts of natural lignin；The aggregate by granular filler and
Powder filler forms, and the percentage by weight of granular filler is 25%, and the percentage by weight of powder filler is 75%；The granular filler
For the glass particle and quartz sand particle that particle size is 5-60 mesh, the ratio of weight and number of glass particle and quartz sand particle is 2:
3；The powder filler is the silica flour and heavy carbonic calcium powder that particle size is 160-1200 mesh, and its ratio of weight and number is 1:2.
The resin is epoxy resin；The coupling agent is γ-methacryloxypropyl trimethoxy silane.
The curing agent is made up of the composition of following percentage by weight：AMBN 16%, benzoyl peroxide 21%,
Peroxidating (2 ethyl hexanoic acid) tert-butyl ester 63%.
The antiseptic is using the homogeneous mixture of modified zeolite and crude tourmaline as complex carrier, on complex carrier
Load the nano titanium oxide of selenium nitrogen tungsten codope, in described complex carrier, the weight ratio of modified zeolite and crude tourmaline
For 2: 1.
The preparation method of the antiseptic is：
（1）Isopropyl titanate, isopropanol and triethanolamine are mixed and stirred for 1.5-2 hours and obtain the first solution, wherein metatitanic acid
Isopropyl ester, isopropanol, the volume ratio of triethanolamine are 1:5：0.8；
（2）Selenium powder and oxalic acid are added in deionized water, are uniformly mixing to obtain the second solution, wherein, mole of selenium powder and oxalic acid
Than for 1:3, the mol ratio of selenium powder and isopropyl titanate is 1:15；
（3）Urea and citric acid are added in deionized water, are uniformly mixing to obtain the 3rd solution, wherein, urea and citric acid
Mol ratio is 1:1.5, the mol ratio of urea and isopropyl titanate is 1:20；
（4）Ammonium tungstate and pyrolkigneous liquid are added in deionized water, obtain the 4th solution, wherein, mole of ammonium tungstate and pyrolkigneous liquid
Than for 1:2, the mol ratio of ammonium tungstate and isopropyl titanate is 1:30；
（5）Second solution, the 3rd solution and the 4th solution are mixed into the 4th solution, wherein the volume of the 4th solution is 30ml；
（6）By modified zeolite and crude tourmaline by weight 2：1 mixing, then ultra-fine grinding to average grain diameter are less than 5.0 μm, obtain
To complex carrier；The preparation method of wherein described modified zeolite is：Stellerite ore is eluriated, crushing and processing to 560-
580 mesh；It is acidified using 1g epidesmine 0.1M hydrochloric acid 40ml as ratio, by the epidesmine and 15% sodium chloride after acidifying
Stirring reaction 3 hours under insulation, place 2 hours, washed to neutrality at room temperature, modified zeolite is obtained after drying；
（7）In the presence of ultrasonic wave, the 4th solution is added dropwise in above-mentioned first solution, adds above-mentioned complex carrier,
Continue stir 1-3 hours obtain colloidal sol；
（8）It is put into after obtained colloidal sol is placed into ageing 2~3 days in Muffle furnace, 190 is warming up to 5~10 DEG C/minute of programming rates
~200 DEG C are incubated 3.5~4 hours, then are warming up to 550~580 DEG C of 40~50min of insulation with 12~15 DEG C/heating rate, with stove
It is cooled to and takes out cooling to be at room temperature ground to particle diameter be 200~400nm.
The preparation method of above-mentioned quartzite slate is：
（1）Each raw material is weighed by proportioning, and it is separated；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then add colorant, coupling agent, aggregate,
Natural lignin, it is stirred under vacuum 6~8min of mixing；Curing agent is eventually adding, 6~8min of mixing is stirred under vacuum, obtains compound；
（3）Compound is evenly laid out in template；
（4）Template is sent into vacuum vibration formation pressing machine and vibrates compressing, the vacuum in the vacuum vibration formation pressing machine
Degree control be -0.1~-0.08MPa, and the control of vacuum vibration formation pressing machine working frequency is 50Hz, and the static pressure on pressure head controls
For 30~50kg, 180~300s is suppressed；
（5）After vibration is compressing, solidification for the first time being carried out successively and is solidified for the second time, the temperature of the first time solidification is
60~80 DEG C, 15~20 minutes time；Second of 100 ± 2 DEG C of solidification temperature, hardening time are 10~20 minutes；
（6）After the completion of solidification, the room temperature completely rear sheet material thicknessing machine that enters to be cooled is fixed thick, then enters by water mill polissoir
Row polishing.
Embodiment 2
A kind of antibacterial artificial quartz sheet material, it is made up of the raw material of following parts by weight：88 parts of aggregate, 12 parts of resin, solidification
0.6 part of agent, 0.8 part of coupling agent, 0.1 part of colorant, 1 part of antiseptic, 1 part of natural lignin；The aggregate by granular filler and
Powder filler forms, and the percentage by weight of granular filler is 20%, and the percentage by weight of powder filler is 80%；The granular filler
For the glass particle and quartz sand particle that particle size is 5-60 mesh, the ratio of weight and number of glass particle and quartz sand particle is 2:
3；The powder filler is the silica flour and heavy carbonic calcium powder that particle size is 160-1200 mesh, and its ratio of weight and number is 1:2.
The resin is phenolic resin；The coupling agent is γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane.
The curing agent is made up of the composition of following percentage by weight：AMBN 16%, benzoyl peroxide 21%,
Peroxidating (2 ethyl hexanoic acid) tert-butyl ester 63%.
The antiseptic is using the homogeneous mixture of modified zeolite and crude tourmaline as complex carrier, on complex carrier
Load the nano titanium oxide of selenium nitrogen tungsten codope, in described complex carrier, the weight ratio of modified zeolite and crude tourmaline
For 3: 1.
The preparation method of the antiseptic is：
（1）Isopropyl titanate, isopropanol and triethanolamine are mixed and stirred for 1.5-2 hours and obtain the first solution, wherein metatitanic acid
Isopropyl ester, isopropanol, the volume ratio of triethanolamine are 1:6：0.8；
（2）Selenium powder and oxalic acid are added in deionized water, are uniformly mixing to obtain the second solution, wherein, mole of selenium powder and oxalic acid
Than for 1:3, the mol ratio of selenium powder and isopropyl titanate is 1:15；
（3）Urea and citric acid are added in deionized water, are uniformly mixing to obtain the 3rd solution, wherein, urea and citric acid
Mol ratio is 1:1.5, the mol ratio of urea and isopropyl titanate is 1:20；
（4）Ammonium tungstate and pyrolkigneous liquid are added in deionized water, obtain the 4th solution, wherein, mole of ammonium tungstate and pyrolkigneous liquid
Than for 1:2, the mol ratio of ammonium tungstate and isopropyl titanate is 1:30；
（5）Second solution, the 3rd solution and the 4th solution are mixed into the 4th solution, wherein the volume of the 4th solution is 30ml；
（6）By modified zeolite and crude tourmaline by weight 3：1 mixing, then ultra-fine grinding to average grain diameter are less than 5.0 μm, obtain
To complex carrier；The preparation method of wherein described modified zeolite is：Stellerite ore is eluriated, crushing and processing to 560-
580 mesh；It is acidified using 1g epidesmine 0.1M hydrochloric acid 40ml as ratio, by the epidesmine and 15% sodium chloride after acidifying
Stirring reaction 3 hours under insulation, place 2 hours, washed to neutrality at room temperature, modified zeolite is obtained after drying；
（7）In the presence of ultrasonic wave, the 4th solution is added dropwise in above-mentioned first solution, adds above-mentioned complex carrier,
Continue stir 1-3 hours obtain colloidal sol；
（8）It is put into after obtained colloidal sol is placed into ageing 2~3 days in Muffle furnace, 190 is warming up to 5~10 DEG C/minute of programming rates
~200 DEG C are incubated 3.5~4 hours, then are warming up to 550~580 DEG C of 40~50min of insulation with 12~15 DEG C/heating rate, with stove
It is cooled to and takes out cooling to be at room temperature ground to particle diameter be 200~400nm.
The preparation method of above-mentioned quartzite slate is：（1）Each raw material is weighed by proportioning, and it is separated；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then add colorant, coupling agent, aggregate,
Natural lignin, it is stirred under vacuum 6~8min of mixing；Curing agent is eventually adding, 6~8min of mixing is stirred under vacuum, obtains compound；
（3）Compound is evenly laid out in template；
（4）Template is sent into vacuum vibration formation pressing machine and vibrates compressing, the vacuum in the vacuum vibration formation pressing machine
Degree control be -0.1~-0.08MPa, and the control of vacuum vibration formation pressing machine working frequency is 50Hz, and the static pressure on pressure head controls
For 30~50kg, 180~300s is suppressed；
（5）After vibration is compressing, solidification for the first time being carried out successively and is solidified for the second time, the temperature of the first time solidification is
60~80 DEG C, 15~20 minutes time；Second of 100 ± 2 DEG C of solidification temperature, hardening time are 10~20 minutes；
（6）After the completion of solidification, the room temperature completely rear sheet material thicknessing machine that enters to be cooled is fixed thick, then enters by water mill polissoir
Row polishing.
Embodiment 3
A kind of antibacterial artificial quartz sheet material, it is made up of the raw material of following parts by weight：92 parts of aggregate, 8 parts of resin, solidification
1 part of agent, 1 part of coupling agent, 2 parts of colorant, 3 parts of antiseptic, 2 parts of natural lignin；The aggregate is filled out by granular filler and powder
Material composition, the percentage by weight of granular filler is 30%, and the percentage by weight of powder filler is 70%；The granular filler is particle diameter
Size is the glass particle and quartz sand particle of 5-60 mesh, and the ratio of weight and number of glass particle and quartz sand particle is 2:3；Institute
It is the silica flour and heavy carbonic calcium powder that particle size is 160-1200 mesh to state powder filler, and its ratio of weight and number is 1:2.
The resin is polyurethane resin；The coupling agent is gamma-aminopropyl-triethoxy-silane.
The curing agent is made up of the composition of following percentage by weight：AMBN 16%, benzoyl peroxide 21%,
Peroxidating (2 ethyl hexanoic acid) tert-butyl ester 63%.
The antiseptic is using the homogeneous mixture of modified zeolite and crude tourmaline as complex carrier, on complex carrier
Load the nano titanium oxide of selenium nitrogen tungsten codope, in described complex carrier, the weight ratio of modified zeolite and crude tourmaline
For 2: 1.
The preparation method of the antiseptic is：
（1）Isopropyl titanate, isopropanol and triethanolamine are mixed and stirred for 1.5-2 hours and obtain the first solution, wherein metatitanic acid
Isopropyl ester, isopropanol, the volume ratio of triethanolamine are 1:5：0.8；
（2）Selenium powder and oxalic acid are added in deionized water, are uniformly mixing to obtain the second solution, wherein, mole of selenium powder and oxalic acid
Than for 1:3, the mol ratio of selenium powder and isopropyl titanate is 1:15；
（3）Urea and citric acid are added in deionized water, are uniformly mixing to obtain the 3rd solution, wherein, urea and citric acid
Mol ratio is 1:1.5, the mol ratio of urea and isopropyl titanate is 1:20；
（4）Ammonium tungstate and pyrolkigneous liquid are added in deionized water, obtain the 4th solution, wherein, mole of ammonium tungstate and pyrolkigneous liquid
Than for 1:2, the mol ratio of ammonium tungstate and isopropyl titanate is 1:30；
（5）Second solution, the 3rd solution and the 4th solution are mixed into the 4th solution, wherein the volume of the 4th solution is 30ml；
（6）By modified zeolite and crude tourmaline by weight 2：1 mixing, then ultra-fine grinding to average grain diameter are less than 5.0 μm, obtain
To complex carrier；The preparation method of wherein described modified zeolite is：Stellerite ore is eluriated, crushing and processing to 560-
580 mesh；It is acidified using 1g epidesmine 0.1M hydrochloric acid 40ml as ratio, by the epidesmine and 15% sodium chloride after acidifying
Stirring reaction 3 hours under insulation, place 2 hours, washed to neutrality at room temperature, modified zeolite is obtained after drying；
（7）In the presence of ultrasonic wave, the 4th solution is added dropwise in above-mentioned first solution, adds above-mentioned complex carrier,
Continue stir 1-3 hours obtain colloidal sol；
（8）It is put into after obtained colloidal sol is placed into ageing 2~3 days in Muffle furnace, 190 is warming up to 5~10 DEG C/minute of programming rates
~200 DEG C are incubated 3.5~4 hours, then are warming up to 550~580 DEG C of 40~50min of insulation with 12~15 DEG C/heating rate, with stove
It is cooled to and takes out cooling to be at room temperature ground to particle diameter be 200~400nm.
The preparation method of above-mentioned quartzite slate is：（1）Each raw material is weighed by proportioning, and it is separated；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then add colorant, coupling agent, aggregate,
Natural lignin, it is stirred under vacuum 6~8min of mixing；Curing agent is eventually adding, 6~8min of mixing is stirred under vacuum, obtains compound；
（3）Compound is evenly laid out in template；
（4）Template is sent into vacuum vibration formation pressing machine and vibrates compressing, the vacuum in the vacuum vibration formation pressing machine
Degree control be -0.1~-0.08MPa, and the control of vacuum vibration formation pressing machine working frequency is 50Hz, and the static pressure on pressure head controls
For 30~50kg, 180~300s is suppressed；
（5）After vibration is compressing, solidification for the first time being carried out successively and is solidified for the second time, the temperature of the first time solidification is
60~80 DEG C, 15~20 minutes time；Second of 100 ± 2 DEG C of solidification temperature, hardening time are 10~20 minutes；
（6）After the completion of solidification, the room temperature completely rear sheet material thicknessing machine that enters to be cooled is fixed thick, then enters by water mill polissoir
Row polishing.
Comparative example 1
Based on embodiment 1, the difference is that only：Curing agent is made up of the composition of following percentage by weight in this comparative example：Cross
BP 37%, peroxidating (2 ethyl hexanoic acid) tert-butyl ester 63%.
Comparative example 2
Based on embodiment 1, the difference is that only：Curing agent is made up of the composition of following percentage by weight in this comparative example：It is even
Nitrogen diisoamyl nitrile 16%, peroxidating (2 ethyl hexanoic acid) tert-butyl ester 84%.
Comparative example 3
Based on embodiment 1, the difference is that only：Curing agent is made up of the composition of following percentage by weight in this comparative example：It is even
Nitrogen diisoamyl nitrile 79%, benzoyl peroxide 21%.
Comparative example 4
Based on embodiment 1, the difference is that only：Antiseptic is only used as carrier using modified zeolite in this comparative example.
Comparative example 5
Based on embodiment 1, the difference is that only：Antiseptic is only used as carrier using crude tourmaline in this comparative example.
Comparative example 6
Based on embodiment 1, the difference is that only：In this comparative example on complex carrier load undoped with nanometer titanium dioxide
Titanium.
Test example 1
Artificial quartz in lump obtained by 1-3 of the embodiment of the present invention and comparative example 1-3 is subjected to conventional products performance detection, the examination criteria
For：JC908-2013.
Mohs' hardness arranges from high to low：1=embodiment of embodiment 2>Embodiment 3>Comparative example 3>2=comparative example of comparative example 1；
Mohs' hardness wherein in embodiment 3 reaches 6, and the Mohs' hardness in comparative example 3 is 5.
Compression strength numerical value is higher, illustrates that the anti-pressure ability of sample is stronger, compression strength arranges from high to low：Embodiment 1>
Embodiment 3>Embodiment 2>Comparative example 3>Comparative example 2>Comparative example 1；Compression strength wherein in embodiment 2 is 255.6MPa, right
Compression strength in ratio 3 is 1550MPa.
Bending strength numerical value is higher, illustrates that the bending resistance of sample is stronger, bending strength arranges from high to low：Embodiment
1>Embodiment 3>Embodiment 2>Comparative example 3>Comparative example 2>Comparative example 1；Bending strength wherein in embodiment 2 is 65MPa, contrast
Bending strength in example 3 is 38MPa.
Thermal linear expansion coefficient numerical value is lower, illustrates that the temperature distortion degree of sample is lower, and thermal linear expansion coefficient is from low
Arranged to height：Embodiment 3<Embodiment 1<Embodiment 2<Comparative example 2<Comparative example 3<It is linear in comparative example 1, wherein embodiment 2
Thermal coefficient of expansion is 2.9 × 10-5/ DEG C, the thermal linear expansion coefficient in comparative example 2 is 3.5 × 10-5/℃。
According to detection, 1-3 of embodiment of the present invention artificial quartz stone plate meets the standard, and relative to comparative example 1-
3, the physical detection performance of the artificial quartz stone plate of embodiment 1 to 3 is significantly increased, particularly Mohs' hardness, compression strength
Greatly enhanced with bending strength, thermal linear expansion coefficient numerical value reduces.
Test example 2
Bacteriostatic experiment is carried out by the embodiment of the present invention 1 to 3 and with the artificial quartz in lump prepared by comparative example 4-6, experimental strain is
Staphylococcus aureus, inoculum density are 1.1 × 106Cfu/mL, by testing the logarithmic mean value after contacting elution 24 hours
Antilogarithm determine its fungistatic effect, the results showed that the antibacterial effect of the artificial quartz in lump of the embodiment of the present invention 1 to 3 is obvious
Better than comparative example 4-6.
Embodiment described above only expresses embodiments of the present invention, and its description is more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent substitution or equivalent transformation
Art scheme, it all should fall within the scope and spirit of the invention.
Claims (7)
1. a kind of preparation method of antibacterial artificial quartz sheet material, it is characterised in that comprise the following steps：
（1）Each raw material is weighed by proportioning, and it is separated；The parts by weight of wherein each raw material are as follows：Aggregate 88-92 parts, tree
Fat 8-12 parts, curing agent 0.6-1 parts, coupling agent 0.8-1 parts, colorant 0.1-2 parts, antiseptic 1-3 parts, natural lignin 1-2
Part；The aggregate is made up of granular filler and powder filler, and the percentage by weight of granular filler is 20-30%, the weight of powder filler
Measuring percentage is：70-80%；The granular filler is the glass particle and quartz sand particle that particle size is 5-60 mesh, glass
The ratio of weight and number of grain and quartz sand particle is 2:3；The powder filler be silica flour that particle size is 160-1200 mesh and
Heavy carbonic calcium powder, its ratio of weight and number are 1:2；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then add colorant, coupling agent, aggregate,
Natural lignin, it is stirred under vacuum 6~8min of mixing；Curing agent is eventually adding, 6~8min of mixing is stirred under vacuum, obtains compound；
（3）Compound is evenly laid out in template；
（4）Template is sent into vacuum vibration formation pressing machine and vibrates compressing, the vacuum in the vacuum vibration formation pressing machine
Degree control be -0.1~-0.08MPa, and the control of vacuum vibration formation pressing machine working frequency is 50Hz, and the static pressure on pressure head controls
For 30~50kg, 180~300s is suppressed；
（5）After vibration is compressing, solidification for the first time being carried out successively and is solidified for the second time, the temperature of the first time solidification is
60~80 DEG C, 15~20 minutes time；Second of 100 ± 2 DEG C of solidification temperature, hardening time are 10~20 minutes；
（6）After the completion of solidification, the room temperature completely rear sheet material thicknessing machine that enters to be cooled is fixed thick, then enters by water mill polissoir
Row polishing.
2. the preparation method of antibacterial artificial quartz sheet material as claimed in claim 1, it is characterised in that the resin is selected from ring
One kind in oxygen tree fat, phenolic resin, acrylic resin, polyurethane resin.
3. the preparation method of antibacterial artificial quartz sheet material as claimed in claim 1, it is characterised in that the coupling agent is
γ-methacryloxypropyl trimethoxy silane, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane, N- β (ammonia second
Base)-γ-aminopropyltriethoxy dimethoxysilane, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, N- β (ammonia second
Base)-γ-aminopropyltrimethoxysilane, anilinomethyl triethoxysilane, gamma-aminopropyl-triethoxy-silane, vinyl
One kind in triethoxysilane, vinyltrimethoxy silane and γ-chloropropyl triethoxysilane.
4. the preparation method of antibacterial artificial quartz sheet material as claimed in claim 1, it is characterised in that the curing agent by with
The composition composition of lower percentage by weight：AMBN 16%, benzoyl peroxide 21%, peroxidating (2 ethyl hexanoic acid) tertiary fourth
Ester 63%.
5. the preparation method of antibacterial artificial quartz sheet material as claimed in claim 1, it is characterised in that the antiseptic is to change
Property zeolite and crude tourmaline homogeneous mixture as complex carrier, the nanometer of selenium nitrogen tungsten codope is loaded on complex carrier
Titanium dioxide, in described complex carrier, the weight ratio of modified zeolite and crude tourmaline is（2-3）∶1.
6. the preparation method of antibacterial artificial quartz sheet material as claimed in claim 5, it is characterised in that the system of the antiseptic
Preparation Method is：
（1）Isopropyl titanate, isopropanol and triethanolamine are mixed and stirred for 1.5-2 hours and obtain the first solution, wherein metatitanic acid
Isopropyl ester, isopropanol, the volume ratio of triethanolamine are 1:（5-6）：0.8；
（2）Selenium powder and oxalic acid are added in deionized water, are uniformly mixing to obtain the second solution, wherein, mole of selenium powder and oxalic acid
Than for 1:3, the mol ratio of selenium powder and isopropyl titanate is 1:15；
（3）Urea and citric acid are added in deionized water, are uniformly mixing to obtain the 3rd solution, wherein, urea and citric acid
Mol ratio is 1:1.5, the mol ratio of urea and isopropyl titanate is 1:20；
（4）Ammonium tungstate and pyrolkigneous liquid are added in deionized water, obtain the 4th solution, wherein, mole of ammonium tungstate and pyrolkigneous liquid
Than for 1:2, the mol ratio of ammonium tungstate and isopropyl titanate is 1:30；
（5）Second solution, the 3rd solution and the 4th solution are mixed into the 4th solution, wherein the volume of the 4th solution is 30ml；
（6）By modified zeolite and crude tourmaline by weight（2-3）：1 mixing, then ultra-fine grinding to average grain diameter are less than 5.0 μ
M, obtain complex carrier；
（7）In the presence of ultrasonic wave, the 4th solution is added dropwise in above-mentioned first solution, adds above-mentioned complex carrier,
Continue stir 1-3 hours obtain colloidal sol；
（8）It is put into after obtained colloidal sol is placed into ageing 2~3 days in Muffle furnace, 190 is warming up to 5~10 DEG C/minute of programming rates
~200 DEG C are incubated 3.5~4 hours, then are warming up to 550~580 DEG C of 40~50min of insulation with 12~15 DEG C/heating rate, with stove
It is cooled to and takes out cooling to be at room temperature ground to particle diameter be 200~400nm.
7. the preparation method of antibacterial artificial quartz sheet material as claimed in claim 5, it is characterised in that the modified zeolite
Preparation method is：Stellerite ore is eluriated, crushing and processing to 560-580 mesh；With 1g epidesmine 0.1M hydrochloric acid 40ml
It is acidified for ratio, stirring reaction 3 hours, room temperature decentralization under insulation by the epidesmine after acidifying and 15% sodium chloride
Put 2 hours, wash to neutrality, modified zeolite is obtained after drying.
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