CN107572895A - A kind of preparation method of artificial quartz stone plate - Google Patents
A kind of preparation method of artificial quartz stone plate Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of artificial quartz stone plate, comprise the following steps：（1）Each raw material is weighed by formula ratio；（2）Antiseptic is added in resin, is stirred under vacuum mixing；Then colorant, coupling agent, aggregate 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）It is compressing by being vibrated in template feeding vacuum vibration formation pressing machine；（5）After vibration is compressing, solidification for the first time is carried out successively and is solidified for the second time.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 method of artificial quartz stone plate.
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 artificial quartz stone plate.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of preparation method of artificial quartz stone plate, comprises the following steps：
（1）Each raw material is weighed by formula ratio, and it is separated；The percentage by weight of wherein each raw material is：Aggregate 88-92%,
Resin 5-7%, curing agent 0.7-1%, coupling agent 0.8-1%, colorant 0.1-2%, antiseptic 1-3%；The weight percent of each component
It is 100% than sum；The aggregate is made up of granular filler and powder filler, and the percentage by weight of granular filler is 20-30%,
The percentage by weight of powder filler is：70-80%；The granular filler is the glass particle and quartz that particle size is 5-60 mesh
The ratio of weight and number of sand particle, glass particle and quartz sand particle is 2:3；The powder filler is that particle size is 160-
The silica flour and heavy carbonic calcium powder of 1200 mesh, its ratio of weight and number are 1:2；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then colorant, coupling agent, aggregate are added,
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
70~90 DEG C, 15~20 minutes time；Second of 120 ± 2 DEG C of solidification temperature, hardening time are 10~30 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 is set by water mill polishing
It is standby to be polished.
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.
The present invention rationally designs to aggregate, has both improved the hardness and intensity of sheet material, can imitate lithotome again,
Reduce production cost.
The particle diameter of granular filler in aggregate and powder filler is defined in the present invention, if wherein granular filler and
The particle diameter of powder filler is too thin, can consume substantial amounts of resin, increases cost, and bubble is difficult to discharge formation in process of production
Aperture, influence the quality of artificial quartz in lump.
Further, the resin is made up of the composition of following percentage by weight：Polybutadiene 30%, acrylic tree
Fat 25%, chloro unsaturated polyester resin 45%.
Because quartz crystal relies primarily on resin-bonded, therefore, the quality of resin determines the quality of artificial quartz in lump.Mesh
Before, the artificial quartz in lump of in the market mainly uses unsaturated-resin, and the content of resin is usually 10% or so or higher, is led
Cause it to be also easy to produce cut in use, reduce its surface smoothness, stain resistance, while ageing-resistant especially corrosion resistance
It is poor, xanthochromia can occur after long-term use of, and cause intensity decreases or even crack.The present invention is carried out to the composition of resin
Improve, found by numerous studies, conduct is compounded using polybutadiene, acryl resin, chloro unsaturated polyester resin
Resin, and Reasonable Regulation And Control its consumption proportion, can greatly reduce main in formula influences artificial quartz in lump deformation and aging not
The dosage of saturated resin, so as to improve the intensity of artificial quartz stone plate, production cost is greatly reduced, makes what is produced
Artificial quartz stone plate is unlikely to deform, non-aging.
Further, the coupling agent is γ-methacryloxypropyl trimethoxy silane, γ-(2,3- epoxies third
Oxygen) propyl trimethoxy silicane, N- β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane, N- (β-aminoethyl)-γ-ammonia
Propyl-triethoxysilicane, N- β (aminoethyl)-γ-aminopropyltrimethoxysilane, anilinomethyl triethoxysilane, γ-
Aminopropyl triethoxysilane, VTES, vinyltrimethoxy silane and γ-chloropropyl triethoxy
One kind in silane.
Further, the curing agent is peroxidating (2 ethyl hexanoic acid) tert-butyl ester, methyl ethyl ketone peroxide, benzoyl peroxide first
One kind in tert-butyl acrylate, dibenzoyl peroxide and fat polyamine.
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.
The present invention is used as resin, and closed using polybutadiene, acryl resin, chloro unsaturated polyester resin compounding
Reason regulates and controls its consumption proportion, can greatly reduce the main unsaturated-resin for influenceing artificial quartz in lump deformation and aging in formula
Dosage, so as to improve the intensity of artificial quartz stone plate, production cost is greatly reduced, makes the artificial quartz in lump produced
Sheet material is unlikely to deform, non-aging.
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 artificial quartz stone plate, it is made up of the raw material of following percentage by weight：Aggregate 90%, resin 6%, curing agent
0.8%th, coupling agent 0.9%, colorant 0.3%, antiseptic 2%；The percentage by weight sum of each component is 100%；The aggregate by
Granular filler and powder filler composition, the percentage by weight of granular filler is 25%, and the percentage by weight of powder filler is：75%；
The granular filler is the weight of the glass particle and quartz sand particle that particle size is 5-60 mesh, glass particle and quartz sand particle
It is 2 to measure portion rate:3；The powder filler is the silica flour and heavy carbonic calcium powder that particle size is 160-1200 mesh, its weight
Portion rate is 1:2.
The resin is made up of the composition of following percentage by weight：Polybutadiene 30%, acryl resin 25%, chloro insatiable hunger
With polyester resin 45%.
The coupling agent is γ-methacryloxypropyl trimethoxy silane；The curing agent is peroxidating (2- second
Base caproic acid) tert-butyl ester.
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 colorant, coupling agent, aggregate are added,
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
70~90 DEG C, 15~20 minutes time；Second of 120 ± 2 DEG C of solidification temperature, hardening time are 10~30 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 is set by water mill polishing
It is standby to be polished.
Embodiment 2
A kind of artificial quartz stone plate, it is made up of the raw material of following percentage by weight：Aggregate 88%, resin 6%, curing agent 1%
, coupling agent 1%, colorant 1%, antiseptic 3%；The percentage by weight sum of each component is 100%；The aggregate is by granular filler
Formed with powder filler, the percentage by weight of granular filler is 20%, and the percentage by weight of powder filler is： 80%；The particle
Filler is the ratio of weight and number of the glass particle and quartz sand particle that particle size is 5-60 mesh, glass particle and quartz sand particle
For 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 made up of the composition of following percentage by weight：Polybutadiene 30%, acryl resin 25%, chloro insatiable hunger
With polyester resin 45%.
The coupling agent is γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane；The curing agent is peroxidating first and second
Ketone.
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 colorant, coupling agent, aggregate are added,
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
70~90 DEG C, 15~20 minutes time；Second of 120 ± 2 DEG C of solidification temperature, hardening time are 10~30 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 is set by water mill polishing
It is standby to be polished.
Embodiment 3
A kind of artificial quartz stone plate, it is made up of the raw material of following percentage by weight：Aggregate 92%, resin 5%, curing agent
0.7%th, coupling agent 0.8%, colorant 0.5%, antiseptic 1%；The percentage by weight sum of each component is 100%；The aggregate by
Granular filler and powder filler composition, the percentage by weight of granular filler is 30%, and the percentage by weight of powder filler is：70%；
The granular filler is the weight of the glass particle and quartz sand particle that particle size is 5-60 mesh, glass particle and quartz sand particle
It is 2 to measure portion rate:3；The powder filler is the silica flour and heavy carbonic calcium powder that particle size is 160-1200 mesh, its weight
Portion rate is 1:2.
The resin is made up of the composition of following percentage by weight：Polybutadiene 30%, acryl resin 25%, chloro insatiable hunger
With polyester resin 45%.
The coupling agent is N- β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane；The curing agent is peroxidating
T-butyl perbenzoate.
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 colorant, coupling agent, aggregate are added,
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
70~90 DEG C, 15~20 minutes time；Second of 120 ± 2 DEG C of solidification temperature, hardening time are 10~30 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 is set by water mill polishing
It is standby to be polished.
Comparative example 1
Based on embodiment 1, the difference is that only：Resin is unsaturated polyester resin in this comparative example.
Comparative example 2
Based on embodiment 1, the difference is that only：Resin is made up of the composition of following percentage by weight in this comparative example：Ya Ke
Power resin 55%, chloro unsaturated polyester resin 45%.
Comparative example 3
Based on embodiment 1, the difference is that only：Resin is made up of the composition of following percentage by weight in this comparative example：Poly- fourth
Diene resin 55%, chloro unsaturated polyester resin 45%.
Comparative example 4
Based on embodiment 1, the difference is that only：Resin is made up of the composition of following percentage by weight in this comparative example：Poly- fourth
Diene resin 30%, acryl resin 70%.
Comparative example 5
Based on embodiment 1, the difference is that only：Antiseptic is only used as carrier using modified zeolite in this comparative example.
Comparative example 6
Based on embodiment 1, the difference is that only：Antiseptic is only used as carrier using crude tourmaline in this comparative example.
Comparative example 7
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 1-4 is subjected to conventional products performance detection, the examination criteria
For：JC908-2013.
Mohs' hardness arranges from high to low：Embodiment 2>1=embodiment of embodiment 3>Comparative example 3>Comparative example 2>Comparative example 1>
Comparative example 4；Mohs' hardness wherein in embodiment 3 reaches 7, 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 4>Comparative example 2>Comparative example 1>Comparative example 3；Compression strength wherein in embodiment 2 is
254.8MPa, the compression strength in comparative example 4 is 151 MPa.
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 4>Comparative example 2>Comparative example 3>Comparative example 1；Bending strength wherein in embodiment 2 is
85.8MPa, the bending strength in comparative example 4 is 35MPa.
According to detection, 1-3 of embodiment of the present invention artificial quartz stone plate meets the standard, and relative to comparative example 1-
4, 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.It can be seen that the present invention is using polybutadiene, acryl resin, chloro unsaturated polyester resin
The resin of compounding, compared with omitting any one in comparative example, in the case of resin adds total amount identical, obtained artificial stone
Bending strength, the compression strength of diamond stone sheet material are higher, show that three generates Synergistic.
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 5-7, 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 5-7.
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 artificial quartz stone plate, it is characterised in that it comprises the following steps：
（1）Each raw material is weighed by formula ratio, and it is separated；The percentage by weight of wherein each raw material is：Aggregate 88-92%,
Resin 5-7%, curing agent 0.7-1%, coupling agent 0.8-1%, colorant 0.1-2%, antiseptic 1-3%；The weight percent of each component
It is 100% than sum；The aggregate is made up of granular filler and powder filler, and the percentage by weight of granular filler is 20-30%,
The percentage by weight of powder filler is：70-80%；The granular filler is the glass particle and quartz that particle size is 5-60 mesh
The ratio of weight and number of sand particle, glass particle and quartz sand particle is 2:3；The powder filler is that particle size is 160-
The silica flour and heavy carbonic calcium powder of 1200 mesh, its ratio of weight and number are 1:2；
（2）Antiseptic is added in resin, is stirred under vacuum 6~10min of mixing；Then colorant, coupling agent, aggregate are added,
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
70~90 DEG C, 15~20 minutes time；Second of 120 ± 2 DEG C of solidification temperature, hardening time are 10~30 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 artificial quartz stone plate as claimed in claim 1, it is characterised in that the resin is by following weight
The composition composition of percentage：Polybutadiene 30%, acryl resin 25%, chloro unsaturated polyester resin 45%.
3. the preparation method of artificial quartz stone plate as claimed in claim 1, it is characterised in that the coupling agent is γ-first
Base acryloxypropyl trimethoxy silane, γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane, N- β (aminoethyl)-
γ-aminopropyltriethoxy dimethoxysilane, N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane, N- β (aminoethyl)-γ-
Aminopropyl trimethoxysilane, anilinomethyl triethoxysilane, gamma-aminopropyl-triethoxy-silane, vinyl triethoxyl
One kind in silane, vinyltrimethoxy silane and γ-chloropropyl triethoxysilane.
4. the preparation method of artificial quartz stone plate as claimed in claim 1, it is characterised in that the curing agent is peroxidating
(2 ethyl hexanoic acid) tert-butyl ester, methyl ethyl ketone peroxide, peroxidized t-butyl perbenzoate, dibenzoyl peroxide and fat polyamine
In one kind.
5. the preparation method of artificial quartz stone plate as claimed in claim 1, it is characterised in that the antiseptic is boiled with modified
The homogeneous mixture of stone and crude tourmaline is as complex carrier, the nano-silica of load selenium nitrogen tungsten codope on complex carrier
Change titanium, in described complex carrier, the weight ratio of modified zeolite and crude tourmaline is（2-3）∶1.
6. the preparation method of artificial quartz stone plate as claimed in claim 5, it is characterised in that the preparation side of the antiseptic
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 artificial quartz stone plate as claimed in claim 5, it is characterised in that the preparation of the modified zeolite
Method is：Stellerite ore is eluriated, crushing and processing to 560-580 mesh；Using 1g epidesmines 0.1M hydrochloric acid 40ml as than
Example be acidified, by the epidesmine after acidifying and 15% sodium chloride under insulation stirring reaction 3 hours, place 2 at room temperature
Hour, wash to neutrality, modified zeolite is obtained after drying.
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| CN108395141A (en) * | 2018-05-07 | 2018-08-14 | 山东大唐宅配家居有限公司 | Artificial quartz stone plate and preparation method thereof with Mount Taishan black jade powder |
| CN109053026A (en) * | 2018-07-23 | 2018-12-21 | 南安市奥力石业有限公司 | A kind of manufacture craft and its making step of artificial stone |
| CN109081674A (en) * | 2018-07-23 | 2018-12-25 | 南安市奥力石业有限公司 | A kind of artificial stone and its production method |
| CN111099854A (en) * | 2019-12-19 | 2020-05-05 | 佛山欧神诺陶瓷有限公司 | Baking-free brick for architectural decoration and preparation method thereof |
| CN113105158A (en) * | 2021-03-08 | 2021-07-13 | 江西理工大学 | Method for recovering quartz from tungsten tailings and preparing artificial stone |
| CN113651561A (en) * | 2021-07-16 | 2021-11-16 | 清远金谷智联环保产业研究院有限公司 | Method for preparing sintering-free artificial synthetic plate by adopting nickel smelting furnace slag |
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| CN113651561A (en) * | 2021-07-16 | 2021-11-16 | 清远金谷智联环保产业研究院有限公司 | Method for preparing sintering-free artificial synthetic plate by adopting nickel smelting furnace slag |
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Application publication date: 20180112 |