A kind of preparation method for strengthening environmentally friendly diatom ooze coating
Technical field
The invention belongs to chemical field of polymer material preparing technology, more particularly to a kind of environmentally friendly diatom ooze coating of enhancing
Preparation method.
Background technology
With the continuous improvement of people's living standards, the requirement to domestic environment is also increasingly paid attention to, for the dress in house
Effect after repairing and fitting up also is paid close attention to.A kind of green inner wall decoration wall material using diatomite as main raw material(s) of diatom ooze.
It, which has, eliminates the work(such as formaldehyde, purification air, regulation humidity, releasing negative oxygen ion, fire protection flame retarding, the self-cleaning, deodorization and sterilization of metope
Energy.But the aggregate that the making of existing diatom ooze decorative wall material uses is quartz or dolomite, and specific surface area is small, absorb-discharge humid
Energy and purification of air performance are all very low.The anti-crack fiber of existing product intensity deficiency, is coated onto on wall over time because plasticity is big
It will ftracture.And the easy mould growth of cellulose fibre, the antiseptic used is calcium hydroxide, calcium hydroxide and two in air
Carbonoxide slow reaction generates calcium carbonate, anti-microbial property will be lost after certain time, although the vapor partial pressure of organic antibacterial agent
It is smaller, but also have certain toxicity, IAQ can be influenceed.Also it is exactly to show product merely using diatomite as formaldehyde catching
Agent, kieselguhr adsorption are desorption and the homeostasis process of absorption, are also being discharged while absorption.Therefore say at present in reality
The diatom ooze decorative wall material of middle application is less desirable.
Patent of invention CN201310628130.5, a kind of Ecological diatom ooze decorative wall material, by diatomite, inorganic pigment,
Calcined zeolite, ethene-vinyl acetate redispersible rubber powder, attapulgite powder, tourmaline load nano-titanium dioxide, polyester are fine
Dimension, adipic dihydrazide etc. mix.The primary functional components of the invention are diatomite, because diatomite has porous knot
Structure, there is heat-insulation and heat-preservation function, the relative humidity of the interior space can be made to be automatically adjusted in 40%~70%;The tourmaline of use
Anion caused by load nano-titanium dioxide has sterilizing function, adsorbable resolving harmful gas, using calcined zeolite conduct
Aggregate, it is because it has the characteristics of loose structure, specific surface area is big, improves moisture adsorption and releasing and purify the function of air;Using
Polyester fiber adds intensity, improves anti-crack ability, and will not go mouldy as anti-crack fiber;Use calcium perborate for
Bactericide is long-acting nontoxic.Solve the problems, such as that existing decoration wall material is present, and method is simple, it is easy to implement..
Patent of invention CN201510888573.7, a kind of new liquid diatom ooze wall material and preparation method thereof, the wall material
It is made up of the composition of following mass fraction:Diatomite 35 ~ 45%, mesohole nano-titanium dioxide 15 ~ 20%, new sustained release glass
Microballoon 5 ~ 8%, Paris white 3.5 ~ 10%, plant cellulose 2 ~ 3%, defoamer 0.1 ~ 0.3%, deionized water surplus.The preparation
Method is using modification of the sodium alginate to sustained release glass microsphere surface so that and microballoon has good dispersiveness in the base, and
Sodium alginate also acts as the effect of dispersant and binding agent in wall material, and without another bonus point powder and binding agent, not only environmental protection is gone back
Save the energy;Also, the release fragrance that glass microsphere can be permanent is sustained, makes wall material that there is long-term bactericidal, insect prevention to prevent
It is mould and other effects, solve the drawbacks of diatom ooze wall material hygroscopicity is big, easily mouldy.In addition, new liquid made from the preparation method
Diatom ooze wall material, has a permanent storage stability, not stratified in Storage period, and storage and transport are easy in gel..
Patent of invention CN201510574339.7, a kind of environmentally friendly diatom ooze composite and preparation method thereof, by diatomite
30 ~ 50%, dicalcium powder 3 ~ 12%, quartz sand 8 ~ 20%, pH adjusting agent 10 ~ 15%, calcined kaolin 6 ~ 10%, talcum powder 4 ~
10%th, sepiolite 5 ~ 10%, pigment 2 ~ 5%, pre-gelatinized starch 2 ~ 4%, hydroxypropyl methyl cellulose 1 ~ 3%, dispersibility breast
Glue 1 ~ 2%, starch ether 1 ~ 2%, sodium tripolyphosphate 0.5 ~ 2%, calgon 0.5 ~ 2%, polyvinyl alcohol 0.5 ~ 1%, Guar
Glue 0.1 ~ 0.5% and nano titanium oxide 0.1 ~ 3% form.The invention preparation method is simple, and construction is easy, and diatomite is porous
Material, can adsorb with the harmful substance such as decomposing formaldehyde, toluene, while there is humidity conditioning function, remove odor function.
In the prior art, the diatom ooze of preparation possesses miscellaneous function, but it is low wearability to be still present, is harmful to
The shortcomings of gas formaldehyde burst size is more, and detergent power is weak.
The content of the invention
The deficiency existing for the diatom ooze coating for preparing in the prior art, the present invention, which provides, a kind of strengthens environmentally friendly diatom ooze
The preparation method of coating.
The present invention is achieved by the following technical solutions:
A kind of preparation method for strengthening environmentally friendly diatom ooze coating, is prepared by following steps:
First, activation lignin is prepared
(1)Take reed stems and leaves, be ground into reed slag, sprinkle water it is moistened to water content be 60 ~ 70%, add reed slag
The Tween-80 of amount 0.05 ~ 0.15%, packed after well mixed, after inoculation pseudomonas aeruginosa carries out sterile solid culture 2 ~ 3 days,
Cultivation matrix is obtained, then in being inoculated with phoenix tail mushroom on cultivation matrix, is persistently cultivated 12 ~ 16 days, cultivation temperature is maintained at 37 ~ 45
℃;
(2)Take culture ripe and extract the cultivation matrix after phoenix-tail mushroom, be milled to powder, addition acetic acid to pH is 3 ~ 3.5, under normal temperature
45 ~ 60min is reacted, is then filtered to remove solid residue, obtains activating lignin;
2nd, quartz-anion composite granule is prepared
(1)40 ~ 50 parts of water, 0.5 ~ 0.7 part of dispersant, 5040,0.2 ~ 0.3 parts of defoamer A10 are mixed by ratio of weight and the number of copies, first
It is scattered to stir and evenly mix, add powder quartz ore and ball milling is carried out into porcelain mill, control the solid-to-liquid ratio to be(2~5):1, choose ball
Expect that ratio is(3~5):1 Ceramic Balls, sequentially add 0.3% dispersant and 0.1% defoamer, and rotating speed is 70 revs/min, ball milling
Time is 3.0 ~ 4.0h, prepares konilite slurry, then adds hydroxyethyl cellulose, prevents the sedimentation of konilite slurry, obtains
The konilite slurry arrived;
(2)40 ~ 50 parts of water, 5 ~ 10 parts of hydroxy ethyl fiber solution mixing are taken by ratio of weight and the number of copies, by negative ion powder according to solid-to-liquid ratio
For 1:1 ratio adds, and is then transferred to vertical mixing mill, ratio of grinding media to material is(3~5):1 Ceramic Balls, sequentially add 0.3% it is scattered
The defoamer A10 of agent 5040 and 0.1%, 1 ~ 2h of ball milling, obtain anion agent slurry;
(3)It is according to mass ratio by konilite slurry and anion slurry(12~25):1 mixing, is added to sand mill, ratio of grinding media to material
For(3~5):1 zirconium ball 30 ~ 60min of wet grinding, is fitted into centrifuge tube, is washed with deionized 3 ~ 4 times, is air-dried under normal temperature,
Obtain quartz-anion composite granule;
3rd, hyper-branched polyester is prepared
By quality parts ratio, the double [4- of 2,2- are taken(2- hydroxy ethoxies)Phenyl] 20 ~ 30 parts of propane, constant temperature melts in 210 DEG C of oil baths
Melt, trimesic acid is added, with 0.1 ~ 0.5 part of stannous octoate;After 3.0 ~ 5.0h of heating stirring, vacuumize and keep strong stirring
1.0 ~ 2.0h is reacted, reaction is poured into methanol and precipitated, tetrahydrofuran is dissolved in after filtering and is precipitated again in methanol while hot after terminating,
40 ~ 60h is dried at 100 DEG C, obtains hyper-branched polyester solid;
4th, preparing strengthens environmentally friendly diatom ooze coating
By ratio of weight and the number of copies, 10 ~ 15 parts of lignin of activation is taken, quartz -12 ~ 24 parts of anion composite granule, hyper-branched polyester is solid
1 ~ 3 part of body, 6 ~ 10 parts of phenol, 1 ~ 4 part of sodium hydroxide, 10 ~ 12 parts of formaldehyde, 10 ~ 24 parts of water, it is well mixed and adds in reactor,
80 ~ 100 DEG C are warming up to, 1 ~ 2h of isothermal reaction obtains compound, and 20 ~ 46 parts of diatomite, ethoxy are then added in compound
2 ~ 5 parts of cellulose, 5 ~ 10 parts of inorganic pigment, 2 ~ 5 parts of calcium hydroxide, 60 ~ 100min is mixed under 800 ~ 1000rpm, you can
To the environmentally friendly diatom ooze coating of enhancing.
Pseudomonas aeruginosa and phoenix-tail mushroom solid state fermentation reed slag, it can effectively decompose cellulose in reed slag and wooden
Element;Rhamnolipid caused by pseudomonas aeruginosa fermentation can promote decomposition of the phoenix-tail mushroom secretion laccase to reed slag lignin, living
Change and improve methylol, phenolic hydroxyl group, alcoholic extract hydroxyl group content on lignin molecule, so as to improve lignin and the phenolic resin degree of polymerization.
Quartzy main component is silica, has porous performance, can load more negative oxygen ions, adsorbs free formaldehyde
And phenol, while negative ion powder contacts with moisture in air or oxygen, releasing negative oxygen ion after ionizing, and improves air matter
Amount;The many combination hyper-branched polyesters of quartzy loose structure energy, further improve the degree of polymerization of phenolic resin adhesive.Bear from
Sub- addition be 4 ~ 8% between when, purifying formaldehyde rate changes small, but anion between 91 ~ 94%, more than 8% after-purification rate
The Percentage bound of powder and silica flour reduces with the increase of negative ion powder addition, therefore is best with 4 ~ 8%.
Hyper-branched polyester has highly branched molecular structure, and radical species are more, and solubility high viscosity is low, can effectively carry
The polymerization speed of high phenolic resin, improve the intensity of resin glue;The characteristics of its radical species is more simultaneously, can more it combine free
Phenol and formaldehyde, reduce the release of phenol and formaldehyde so as to improve Environmental security;On the other hand, phenolic resin is due to lignin
With the addition of silica flour complex, gel-forming property is influenceed, this influence can be eliminated using hyper-branched polyester.
As a further improvement on the present invention, step 1(1)Described pseudomonas aeruginosa fills liquid prior to activation medium
Measure in the conical flask for 20%, inoculum concentration 5%, 37 DEG C, 12 ~ 16h of activation culture under 200rpm.
As a further improvement on the present invention, the activation medium is prepared by following density component material:Vegetable seed
Oily 30g/L, Dried Corn Steep Liquor Powder 6g/L, NaNO36g/L, K2HPO40.9g/L, NaH2PO40.6g/L, MgSO40.3g/L,
CaCl20.05g/L, NaCl 1.5g/L, adjust pH to 6.5 ~ 7.0.
In best medium, the rhamnolipid average product that pseudomonas aeruginosa ferments to obtain is 30.41 ~ 34.52g/L.
As a further improvement on the present invention, step 2(1)Described powder quartz ore fineness is 200 ~ 300 mesh.
The granule size of konilite determines its dispersive property and absorption property, and granularity is smaller to disperse better but adsorption capacity
It is low, therefore in order to preferably disperse to adsorb negative ion powder simultaneously, the silica flour using 200 ~ 300 mesh is best.
As a further improvement on the present invention, the double [4- of 2,2- described in step 3(2- hydroxy ethoxies)Phenyl] propane with
The mol ratio of benzenetricarboxylic acid is(2~4):1.
The mol ratio of two kinds of monomers influences hyper-branched polyester molecular weight and the dissaving polymer of terminal groups, and 2,2- is double
[4-(2- hydroxy ethoxies)Phenyl] mol ratio of propane and trimesic acid is 2:Terminal groups dispersiveness big poly- can be obtained when 1
Ester, there are more binding sites(Group), so as to promote the intensity of resin reaction polymerization speed and resin, anti-wear performance.
As a further improvement on the present invention, the quartz described in step 4-anion composite granule is consolidated with hyper-branched polyester
Body amount ratio is(8~15):1.
The content of hyper-branched polyester influences resin integrally curing conversion ratio, and content high resin solidification conversion ratio is low, and content is low
Resin bonding strength and anti-wear performance are low, when hyperbranched poly ester content is 5 ~ 15%, the solidification conversion ratio of phenolic resin for 95 ~
98%, anti-wear performance and bond strength rate of change are small, overall resin property are influenceed little.
As a further improvement on the present invention, the viscosity of the hydroxyethyl cellulose described in step 4 is 5000 ~ 8000.
Hydroxyethyl cellulose can play thickening, protection hydrate colloid, the smear strengthened adhesive power, improve slurry
Effect, while the anti-wear performance for improving coating can be combined with hyper-branched polyester, viscosity is too high to accelerate paint adhesion speed.
Beneficial effects of the present invention:
1st, preparation technology of the present invention requires low, it is not necessary to high capital equipment and raw material, has good economic benefit;
2nd, the diatom ooze coating that is prepared into of the present invention is safe and reliable, and burst size of methanal is low, at the same can also discharge beneficial negative oxygen from
Son, environmental pollution is low, meets demand of the people to environment-friendly materials;
3rd, the diatom ooze coating abrasion resistance for preparing of the present invention is high, and curing rate is fast, and bonding strength is high, has excellent water-fast resistance to
Climate performance.
Embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1
First, activation lignin is prepared
(1)Take reed stems and leaves, be ground into reed slag, sprinkle water it is moistened to water content be 60%, add reed slag quality
0.05% Tween-80, pack after well mixed, after inoculation pseudomonas aeruginosa carries out sterile solid culture 2 days, cultivated
Matrix, then in being inoculated with phoenix tail mushroom on cultivation matrix, persistently cultivate 12 days, cultivation temperature is maintained at 37 DEG C;
In the conical flask that described pseudomonas aeruginosa is 20% prior to activation medium liquid amount, inoculum concentration 5%, 37 DEG C,
Activation culture 12h under 200rpm;The activation medium is prepared by following density component material:Rapeseed oil 30g/L, corn
Paste dry powder 6g/L, NaNO36g/L, K2HPO40.9g/L, NaH2PO40.6g/L, MgSO40.3g/L, CaCl20.05g/L,
NaCl 1.5g/L, adjust pH to 6.5;
(2)Take culture ripe and extract the cultivation matrix after phoenix-tail mushroom, be milled to powder, it is 3 to add acetic acid to pH, is reacted under normal temperature
45min, solid residue is then filtered to remove, obtains activating lignin;
2nd, quartz-anion composite granule is prepared
(1)40 parts of water, 0.5 part of dispersant, 5040,0.2 parts of defoamer A10 are mixed by ratio of weight and the number of copies, it is mixed first to disperse stirring
It is even, add the powder quartz ore that fineness is 200 mesh and ball milling is carried out into porcelain mill, it is 2 to control solid-to-liquid ratio:1, choose ball material
Than for 3:1 Ceramic Balls, 0.3% dispersant and 0.1% defoamer are sequentially added, rotating speed is 70 revs/min, Ball-milling Time is
3.0h, konilite slurry is prepared, then adds hydroxyethyl cellulose, prevent the sedimentation of konilite slurry, obtained konilite
Slurry;
(2)40 parts of water, the mixing of 5 parts of hydroxy ethyl fiber solution are taken by ratio of weight and the number of copies, according to solid-to-liquid ratio are 1 by negative ion powder:1
Ratio adds, and is then transferred to vertical mixing mill, ratio of grinding media to material 3:1 Ceramic Balls, sequentially add 0.3% He of dispersant 5040
0.1% defoamer A10, ball milling 1h, obtain anion agent slurry;
(3)According to mass ratio it is 12 by konilite slurry and anion slurry:1 mixing, is added to sand mill, ratio of grinding media to material 3:1
Zirconium ball wet grinding 30min, be fitted into centrifuge tube, be washed with deionized 3 ~ 4 times, under normal temperature air-dry, obtain quartz-bear from
Sub- composite granule;
3rd, hyper-branched polyester is prepared
By quality parts ratio, the double [4- of 2,2- are taken(2- hydroxy ethoxies)Phenyl] 20 parts of propane, constant temperature melts in 210 DEG C of oil baths,
Add trimesic acid(2,2- double [4-(2- hydroxy ethoxies)Phenyl] mol ratio of propane and trimesic acid is 2:1), with 0.1
Part stannous octoate;After heating stirring 3.0h, vacuumize and keep strong stirring to react 1.0h, reaction pours into methanol while hot after terminating
Middle precipitation, tetrahydrofuran is dissolved in after filtering and is precipitated again in methanol, 40h is dried at 100 DEG C, hyper-branched polyester is obtained and consolidates
Body;
4th, preparing strengthens environmentally friendly diatom ooze coating
By ratio of weight and the number of copies, take and activate 10 parts of lignin, quartz -12 parts of anion composite granule, 1 part of hyper-branched polyester solid,
6 parts of phenol, 1 part of sodium hydroxide, 10 parts of formaldehyde, 10 parts of water, it is well mixed and adds in reactor, be warming up to 80 ~ 100 DEG C, constant temperature
Reaction 1h obtains compound, and 20 parts of diatomite, 2 parts of hydroxyethyl cellulose, 5 parts of inorganic pigment, hydrogen are then added in compound
2 parts of calcium oxide, mixes 60min at 800 rpm, you can obtains strengthening environmentally friendly diatom ooze coating.
Embodiment 2
First, activation lignin is prepared
(1)Take reed stems and leaves, be ground into reed slag, sprinkle water it is moistened to water content be 70%, add reed slag quality
0.15% Tween-80, pack after well mixed, after inoculation pseudomonas aeruginosa carries out sterile solid culture 3 days, cultivated
Matrix, then in being inoculated with phoenix tail mushroom on cultivation matrix, persistently cultivate 16 days, cultivation temperature is maintained at 45 DEG C;
In the conical flask that described pseudomonas aeruginosa is 20% prior to activation medium liquid amount, inoculum concentration 5%, 37 DEG C,
Activation culture 16h under 200rpm;The activation medium is prepared by following density component material:Rapeseed oil 30g/L, corn
Paste dry powder 6g/L, NaNO36g/L, K2HPO40.9g/L, NaH2PO40.6g/L, MgSO40.3g/L, CaCl20.05g/L,
NaCl 1.5g/L, adjust pH to 7.0
(2)Take culture ripe and extract the cultivation matrix after phoenix-tail mushroom, be milled to powder, addition acetic acid to pH is 3.5, anti-under normal temperature
60min is answered, is then filtered to remove solid residue, obtains activating lignin;
2nd, quartz-anion composite granule is prepared
(1)50 parts of water, 0.7 part of dispersant, 5040,0.3 parts of defoamer A10 are mixed by ratio of weight and the number of copies, it is mixed first to disperse stirring
It is even, add the powder quartz ore that fineness is 300 mesh and ball milling is carried out into porcelain mill, it is 5 to control solid-to-liquid ratio:1, choose ball material
Than for 5:1 Ceramic Balls, 0.3% dispersant and 0.1% defoamer are sequentially added, rotating speed is 70 revs/min, Ball-milling Time is
4.0h, konilite slurry is prepared, then adds hydroxyethyl cellulose, prevent the sedimentation of konilite slurry, obtained konilite
Slurry;
(2)50 parts of water, the mixing of 10 parts of hydroxy ethyl fiber solution are taken by ratio of weight and the number of copies, according to solid-to-liquid ratio are 1 by negative ion powder:1
Ratio add, be then transferred to vertical mixing mill, ratio of grinding media to material 5:1 Ceramic Balls, sequentially add 0.3% He of dispersant 5040
0.1% defoamer A10, ball milling 2h, obtain anion agent slurry;
(3)According to mass ratio it is 25 by konilite slurry and anion slurry:1 mixing, is added to sand mill, ratio of grinding media to material 5:1
Zirconium ball wet grinding 60min, be fitted into centrifuge tube, be washed with deionized 3 ~ 4 times, under normal temperature air-dry, obtain quartz-bear from
Sub- composite granule;
3rd, hyper-branched polyester is prepared
By quality parts ratio, the double [4- of 2,2- are taken(2- hydroxy ethoxies)Phenyl] 30 parts of propane, constant temperature melts in 210 DEG C of oil baths,
Add trimesic acid(2,2- double [4-(2- hydroxy ethoxies)Phenyl] mol ratio of propane and trimesic acid is 2:1), with 0.5
Part stannous octoate;After heating stirring 5.0h, vacuumize and keep strong stirring to react 2.0h, reaction pours into methanol while hot after terminating
Middle precipitation, tetrahydrofuran is dissolved in after filtering and is precipitated again in methanol, 60h is dried at 100 DEG C, hyper-branched polyester is obtained and consolidates
Body;
4th, preparing strengthens environmentally friendly diatom ooze coating
By ratio of weight and the number of copies, take and activate 15 parts of lignin, quartz -24 parts of anion composite granule, 3 parts of hyper-branched polyester solid,
10 parts of phenol, 4 parts of sodium hydroxide, 12 parts of formaldehyde, 24 parts of water, it is well mixed and adds in reactor, be warming up to 100 DEG C, constant temperature is anti-
Answer 2h to obtain compound, 46 parts of diatomite, 5 parts of hydroxyethyl cellulose, 10 parts of inorganic pigment, hydrogen-oxygen are then added in compound
Change 5 parts of calcium, mix 100min under 1000rpm, you can obtain strengthening environmentally friendly diatom ooze coating.
Embodiment 3
First, activation lignin is prepared
(1)Take reed stems and leaves, be ground into reed slag, sprinkle water it is moistened to water content be 65%, add reed slag quality
0.1% Tween-80, packed after well mixed, after inoculation pseudomonas aeruginosa carries out sterile solid culture 3 days, obtain cultivation base
Matter, then in being inoculated with phoenix tail mushroom on cultivation matrix, persistently cultivate 14 days, cultivation temperature is maintained at 40 DEG C;
In the conical flask that described pseudomonas aeruginosa is 20% prior to activation medium liquid amount, inoculum concentration 5%, 37 DEG C,
Activation culture 14h under 200rpm;The activation medium is prepared by following density component material:Rapeseed oil 30g/L, corn
Paste dry powder 6g/L, NaNO36g/L, K2HPO40.9g/L, NaH2PO40.6g/L, MgSO40.3g/L, CaCl20.05g/L,
NaCl 1.5g/L, adjust pH to 6.5 ~ 7.0
(2)Take culture ripe and extract the cultivation matrix after phoenix-tail mushroom, be milled to powder, addition acetic acid to pH is 3.3, anti-under normal temperature
50min is answered, is then filtered to remove solid residue, obtains activating lignin;
2nd, quartz-anion composite granule is prepared
(1)45 parts of water, 0.6 part of dispersant, 5040,0.25 parts of defoamer A10 are mixed by ratio of weight and the number of copies, it is mixed first to disperse stirring
It is even, add the powder quartz ore that fineness is 220 mesh and ball milling is carried out into porcelain mill, it is 3 to control solid-to-liquid ratio:1, choose ball material
Than for 4:1 Ceramic Balls, 0.3% dispersant and 0.1% defoamer are sequentially added, rotating speed is 70 revs/min, Ball-milling Time is
3.5h, konilite slurry is prepared, then adds hydroxyethyl cellulose, prevent the sedimentation of konilite slurry, obtained konilite
Slurry;
(2)45 parts of water, the mixing of 8 parts of hydroxy ethyl fiber solution are taken by ratio of weight and the number of copies, according to solid-to-liquid ratio are 1 by negative ion powder:1
Ratio adds, and is then transferred to vertical mixing mill, ratio of grinding media to material 4:1 Ceramic Balls, sequentially add 0.3% He of dispersant 5040
0.1% defoamer A10, ball milling 1.5h, obtain anion agent slurry;
(3)According to mass ratio it is 20 by konilite slurry and anion slurry:1 mixing, is added to sand mill, ratio of grinding media to material 4:1
Zirconium ball wet grinding 50min, be fitted into centrifuge tube, be washed with deionized 3 ~ 4 times, under normal temperature air-dry, obtain quartz-bear from
Sub- composite granule;
3rd, hyper-branched polyester is prepared
By quality parts ratio, the double [4- of 2,2- are taken(2- hydroxy ethoxies)Phenyl] 25 parts of propane, constant temperature melts in 210 DEG C of oil baths,
Add trimesic acid(2,2- double [4-(2- hydroxy ethoxies)Phenyl] mol ratio of propane and trimesic acid is 2:1), with 0.4
Part stannous octoate;After heating stirring 4.0h, vacuumize and keep strong stirring to react 1.5h, reaction pours into methanol while hot after terminating
Middle precipitation, tetrahydrofuran is dissolved in after filtering and is precipitated again in methanol, 50h is dried at 100 DEG C, hyper-branched polyester is obtained and consolidates
Body;
4th, preparing strengthens environmentally friendly diatom ooze coating
By ratio of weight and the number of copies, take and activate 12 parts of lignin, quartz -18 parts of anion composite granule, 2 parts of hyper-branched polyester solid,
8 parts of phenol, 2 parts of sodium hydroxide, 11 parts of formaldehyde, 17 parts of water, it is well mixed and adds in reactor, be warming up to 80 ~ 100 DEG C, constant temperature
Reaction 2h obtains compound, and 22 parts of diatomite, 3 parts of hydroxyethyl cellulose, 5 parts of inorganic pigment, hydrogen are then added in compound
3 parts of calcium oxide, 80min is mixed under 900rpm, you can obtains strengthening environmentally friendly diatom ooze coating.
Embodiment 4
First, activation lignin is prepared
(1)Take reed stems and leaves, be ground into reed slag, sprinkle water it is moistened to water content be 62%, add reed slag quality
0.15% Tween-80, pack after well mixed, after inoculation pseudomonas aeruginosa carries out sterile solid culture 2 days, cultivated
Matrix, then in being inoculated with phoenix tail mushroom on cultivation matrix, persistently cultivate 16 days, cultivation temperature is maintained at 40 DEG C;
In the conical flask that described pseudomonas aeruginosa is 20% prior to activation medium liquid amount, inoculum concentration 5%, 37 DEG C,
Activation culture 12h under 200rpm;The activation medium is prepared by following density component material:Rapeseed oil 30g/L, corn
Paste dry powder 6g/L, NaNO36g/L, K2HPO40.9g/L, NaH2PO40.6g/L, MgSO40.3g/L, CaCl20.05g/L,
NaCl 1.5g/L, adjust pH to 6.5 ~ 7.0
(2)Take culture ripe and extract the cultivation matrix after phoenix-tail mushroom, be milled to powder, addition acetic acid to pH is 3.3, anti-under normal temperature
50min is answered, is then filtered to remove solid residue, obtains activating lignin;
2nd, quartz-anion composite granule is prepared
(1)42 parts of water, 0.5 part of dispersant, 5040,0.3 parts of defoamer A10 are mixed by ratio of weight and the number of copies, it is mixed first to disperse stirring
It is even, add the powder quartz ore that fineness is 220 mesh and ball milling is carried out into porcelain mill, it is 2 to control solid-to-liquid ratio:1, choose ball material
Than for 5:1 Ceramic Balls, 0.3% dispersant and 0.1% defoamer are sequentially added, rotating speed is 70 revs/min, Ball-milling Time is
3.0h, konilite slurry is prepared, then adds hydroxyethyl cellulose, prevent the sedimentation of konilite slurry, obtained konilite
Slurry;
(2)40 parts of water, the mixing of 10 parts of hydroxy ethyl fiber solution are taken by ratio of weight and the number of copies, according to solid-to-liquid ratio are 1 by negative ion powder:1
Ratio add, be then transferred to vertical mixing mill, ratio of grinding media to material 5:1 Ceramic Balls, sequentially add 0.3% He of dispersant 5040
0.1% defoamer A10, ball milling 2.0h, obtain anion agent slurry;
(3)According to mass ratio it is 15 by konilite slurry and anion slurry:1 mixing, is added to sand mill, ratio of grinding media to material 5:1
Zirconium ball wet grinding 60min, be fitted into centrifuge tube, be washed with deionized 3 ~ 4 times, under normal temperature air-dry, obtain quartz-bear from
Sub- composite granule;
3rd, hyper-branched polyester is prepared
By quality parts ratio, the double [4- of 2,2- are taken(2- hydroxy ethoxies)Phenyl] 25 parts of propane, constant temperature melts in 210 DEG C of oil baths,
Add trimesic acid(2,2- double [4-(2- hydroxy ethoxies)Phenyl] mol ratio of propane and trimesic acid is 2:1), with 0.4
Part stannous octoate;After heating stirring 5.0h, vacuumize and keep strong stirring to react 1.0h, reaction pours into methanol while hot after terminating
Middle precipitation, tetrahydrofuran is dissolved in after filtering and is precipitated again in methanol, 40h is dried at 100 DEG C, hyper-branched polyester is obtained and consolidates
Body;
4th, preparing strengthens environmentally friendly diatom ooze coating
By ratio of weight and the number of copies, take and activate 12 parts of lignin, quartz -20 parts of anion composite granule, 2 parts of hyper-branched polyester solid,
8 parts of phenol, 2 parts of sodium hydroxide, 10 parts of formaldehyde, water 15, it is well mixed and adds in reactor, be warming up to 80 ~ 100 DEG C, constant temperature is anti-
Answer 1.5h to obtain compound, 22 parts of diatomite, 3 parts of hydroxyethyl cellulose, 10 parts of inorganic pigment, hydrogen are then added in compound
5 parts of calcium oxide, 100min is mixed under 1000rpm, you can obtains strengthening environmentally friendly diatom ooze coating.
Embodiment 5
First, activation lignin is prepared
(1)Take reed stems and leaves, be ground into reed slag, sprinkle water it is moistened to water content be 65%, add reed slag quality
0.15% Tween-80, pack after well mixed, after inoculation pseudomonas aeruginosa carries out sterile solid culture 3 days, cultivated
Matrix, then in being inoculated with phoenix tail mushroom on cultivation matrix, persistently cultivate 16 days, cultivation temperature is maintained at 40 DEG C;
In the conical flask that described pseudomonas aeruginosa is 20% prior to activation medium liquid amount, inoculum concentration 5%, 37 DEG C,
Activation culture 12h under 200rpm;The activation medium is prepared by following density component material:Rapeseed oil 30g/L, corn
Paste dry powder 6g/L, NaNO36g/L, K2HPO40.9g/L, NaH2PO40.6g/L, MgSO40.3g/L, CaCl20.05g/L,
NaCl 1.5g/L, adjust pH to 6.5;
(2)Take culture ripe and extract the cultivation matrix after phoenix-tail mushroom, be milled to powder, addition acetic acid to pH is 3.5, anti-under normal temperature
60min is answered, is then filtered to remove solid residue, obtains activating lignin;
2nd, quartz-anion composite granule is prepared
(1)45 parts of water, 0.7 part of dispersant, 5040,0.3 parts of defoamer A10 are mixed by ratio of weight and the number of copies, it is mixed first to disperse stirring
It is even, add the powder quartz ore that fineness is 300 mesh and ball milling is carried out into porcelain mill, it is 4 to control solid-to-liquid ratio:1, choose ball material
Than for 4:1 Ceramic Balls, 0.3% dispersant and 0.1% defoamer are sequentially added, rotating speed is 70 revs/min, Ball-milling Time is
4.0h, konilite slurry is prepared, then adds hydroxyethyl cellulose, prevent the sedimentation of konilite slurry, obtained konilite
Slurry;
(2)45 parts of water, the mixing of 10 parts of hydroxy ethyl fiber solution are taken by ratio of weight and the number of copies, according to solid-to-liquid ratio are 1 by negative ion powder:1
Ratio add, be then transferred to vertical mixing mill, ratio of grinding media to material 5:1 Ceramic Balls, sequentially add 0.3% He of dispersant 5040
0.1% defoamer A10, ball milling 2h, obtain anion agent slurry;
(3)According to mass ratio it is 15 by konilite slurry and anion slurry:1 mixing, is added to sand mill, ratio of grinding media to material 3:1
Zirconium ball wet grinding 50min, be fitted into centrifuge tube, be washed with deionized 3 ~ 4 times, under normal temperature air-dry, obtain quartz-bear from
Sub- composite granule;
3rd, hyper-branched polyester is prepared
By quality parts ratio, the double [4- of 2,2- are taken(2- hydroxy ethoxies)Phenyl] 30 parts of propane, constant temperature melts in 210 DEG C of oil baths,
Add trimesic acid(2,2- double [4-(2- hydroxy ethoxies)Phenyl] mol ratio of propane and trimesic acid is 2:1), with 0.5
Part stannous octoate;After heating stirring 4.0h, vacuumize and keep strong stirring to react 2.0h, reaction pours into methanol while hot after terminating
Middle precipitation, tetrahydrofuran is dissolved in after filtering and is precipitated again in methanol, 48h is dried at 100 DEG C, hyper-branched polyester is obtained and consolidates
Body;
4th, preparing strengthens environmentally friendly diatom ooze coating
By ratio of weight and the number of copies, take and activate 15 parts of lignin, quartz -18 parts of anion composite granule, 2 parts of hyper-branched polyester solid,
8 parts of phenol, 2 parts of sodium hydroxide, 12 parts of formaldehyde, 22 parts of water, it is well mixed and adds in reactor, be warming up to 90 DEG C, isothermal reaction
1.5h obtains compound, and 44 parts of diatomite, 4 parts of hydroxyethyl cellulose, 8 parts of inorganic pigment, hydrogen-oxygen are then added in compound
Change 5 parts of calcium, mix 100min under 1000rpm, you can obtain strengthening environmentally friendly diatom ooze coating.
Diatom ooze coating prepared by comprehensive detection embodiment 1 ~ 5, its performance such as table 1.
Table 1 strengthens environmentally friendly diatom ooze coating performance table
As shown in Table 1, the environmentally friendly diatom ooze coating that prepared by the present invention meets safe mark, has good performance and purification of air
Ability.
Above example is only the exemplary embodiment of the present invention, is not used in the limitation present invention, protection scope of the present invention
It is defined by the claims.Those skilled in the art can make various repair to the present invention in the essence and protection domain of the present invention
Change or equivalent substitution, this modification or equivalent substitution also should be regarded as being within the scope of the present invention.