CN110204972A - A kind of preparation method of absorbent-type environmental protection coating material - Google Patents

A kind of preparation method of absorbent-type environmental protection coating material Download PDF

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CN110204972A
CN110204972A CN201910637459.5A CN201910637459A CN110204972A CN 110204972 A CN110204972 A CN 110204972A CN 201910637459 A CN201910637459 A CN 201910637459A CN 110204972 A CN110204972 A CN 110204972A
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chitosan
absorbent
environmental protection
coating material
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吴波
王成兵
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/06—Making microcapsules or microballoons by phase separation
    • B01J13/14—Polymerisation; cross-linking
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/20—After-treatment of capsule walls, e.g. hardening
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Wood Science & Technology (AREA)
  • Dispersion Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The present invention relates to technical field of coatings, more particularly, to a kind of preparation method of absorbent-type environmental protection coating material.Absorption particle is first prepared, then acrylic resin is dissolved in aqueous acetone solution, levelling agent and defoaming agent is added, add absorption particle and stirs to obtain component A；Curing agent is added in ethyl acetate and is uniformly mixed to obtain B component；Absorbent-type environmental protection coating material is stirred evenly to obtain after component A is mixed with B component.Absorption particle PARA FORMALDEHYDE PRILLS(91,95) pernicious gas in coating of the present invention has biggish adsorption capacity, it is not easy to reach adsorption saturation state.

Description

A kind of preparation method of absorbent-type environmental protection coating material
Technical field
The present invention relates to technical field of coatings, more particularly, to a kind of preparation method of absorbent-type environmental protection coating material.
Background technique
As the improvement of people's living standards, interior decoration is increasingly becoming the topic being concerned, and part decorations institute Material can discharge poisonous and hazardous substance, to cause the pollution of indoor environment, endanger human health.Indoor environment Pollution with the most serious after fitting up of new residence, after fitting up of new residence the most common chemical contamination gas include formaldehyde, benzene homologues, ammonia, Radon gas and volatile organic matter etc., this five kinds of toxic gases and harmful substance are referred to as 5 big stealths in house fitting and kill Hand.Wherein formaldehyde is carcinogenic substance, has been listed in the detection project of China's building decoration engineering compulsory execution.In order in clean room Air, purifying formaldehyde coating come into being, and with the features such as at low cost, coated area is big, are suitble to large-scale use.
China Patent Publication No. CN105802425 discloses a kind of environment-friendly antibacterial interior wall coating containing conch meal, the painting By addition conch meal in material, adsorbed using the porous structure PARA FORMALDEHYDE PRILLS(91,95) of conch meal, although can PARA FORMALDEHYDE PRILLS(91,95) have it is certain Suction-operated, but the adsorption capacity of conch meal is small, easily reaches saturation state to the formaldehyde absorbing in air, causes first The persistence of aldehyde absorption is poor；China Patent Publication No. CN102277050 discloses a kind of environment-friendly water-based interior wall of function of removing formaldehyde Coating and preparation method thereof will carry out ultra-fine grinding containing the formaldehyde adsorption resin of amino, imdazole derivatives functional group, by formaldehyde Absorption resin, which is added to, is prepared into the interior wall coating with suction-operated in water paint, since resin porosity is poor, PARA FORMALDEHYDE PRILLS(91,95) Suction-operated it is weak, effect is not obvious；It is difunctional that China Patent Publication No. CN103468049 discloses a kind of hole adsorption-decomposition function Except the coating and preparation method thereof of formaldehyde, carrier using sepiolite as photochemical catalyst titanium dioxide, and it is excellent using its The pernicious gases such as cellular structure PARA FORMALDEHYDE PRILLS(91,95) adsorbed, but it is small to capacity of pernicious gas absorption, it is necessary to have illumination Under conditions of to could PARA FORMALDEHYDE PRILLS(91,95) decompose, realize the recovery of the adsorption capacity of PARA FORMALDEHYDE PRILLS(91,95), and interior is difficult to see sunlight, institute Interior is used for except formaldehyde is subject to certain restrictions with it.
Summary of the invention
The present invention is to be easy the problem of reaching saturation in order to overcome prior art formaldehyde adsorbent adsorption capacity small, provide A kind of preparation method of absorbent-type environmental protection coating material.
To achieve the goals above, the invention adopts the following technical scheme: a kind of preparation method of absorbent-type environmental protection coating material, The following steps are included:
1) concentration is added in chitosan and ammonium chloride is in 1-3wt% aqueous acetic acid, and emulsifier tween 80 is added in stirring and dissolving It is uniformly mixed to obtain mixed liquor, mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, it is 2- that concentration, which is added, in condensation microballoon 5wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 1-3h, filters, and complex microsphere is dried to obtain in washing at room temperature；By ammonium hydroxide, Deionized water and ethyl alcohol mix to obtain mixed liquor, and complex microsphere is added, and tetraethyl orthosilicate is then added dropwise into mixed liquor, are aged 5- 10h, centrifuge separation, drying at room temperature obtain silica-chitosan complex microsphere；Silica-chitosan complex microsphere is placed in It is heated to 600-650 DEG C in crucible, calcines 3-5h, is cooled to room temperature to obtain absorption particle；
2) acrylic resin is dissolved in aqueous acetone solution, levelling agent and defoaming agent is added, 1- is stirred with 300-500r/min 2h；
3) absorption particle is added into the material of step 2), component A is obtained with 100-200r/min stirring 20-30min；
4) curing agent is added in ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
The present invention under the action of crosslinking agent using being first prepared into chitosan compound microsphere, chitosan microball using chitosan In be wrapped in partial oxidation ammonium；Hydrolysis production silica, silica occur under alkaline condition for tetraethyl orthosilicate It is deposited to chitosan compound microsphere surface, so that layer of silicon dioxide layer is deposited on chitosan compound microsphere surface, finally in height It is calcined under the conditions of temperature, silica layer surface forms the through-hole of dispersion, the chitosan microball coated inside silicon dioxide layer It is carbonized at high temperature, being formed has more lacunose carbonization chitosan microball, due to the chitosan microball voidage of carbonization It is higher, and silica interior has biggish space, can accommodate enough carbonization chitosans, so having to pernicious gas There is stronger and lasting absorption property, it is not easy to reach saturation state.
The surface coated silicon dioxide layer of chitosan compound microsphere plays the role of two, first is that utilizing the gap energy on its surface It is enough that auxiliary suction-operated is played to pernicious gas formaldehyde；Second is that silicon dioxide layer can play protection to internal carbonization chitosan Effect forms protective layer on carbonization chitosan surface, prevents from causing under coating agitating procedure or the effects of by external force collision The breaking deformation of carbonization chitosan.
In high-temperature burning process, mixed ammonium chloride decomposes ammonification under the high temperature conditions inside chitosan compound microsphere Gas escapes, the active force escaped in chitosan carbonisation by gas, to form the carbonization of macropore from chitosan inside The common chitosan of the aperture ratio aperture to be formed that is carbonized of chitosan, carbonization chitosan surface is big, to increase in carbonization chitosan Its adsorption capacity and adsorption rate to pernicious gas is improved in the space in portion.
Preferably, the mass ratio of chitosan and ammonium chloride is 1:0.1-0.2 in the step 1).
Preferably, condensation water includes sodium hydroxide, methanol and deionized water in the step 1)；The quality of the three Than for 1:2-3:5-6.
Preferably, the mass ratio of complex microsphere and tetraethyl orthosilicate is 1:2-3 in the step 1).
Preferably, in the step 1) chitosan into cross modification, method of modifying the following steps are included:
Rodlike titanium dioxide granule is dispersed in dehydrated alcohol, suspension is obtained with 800-1000r/min stirring 2-3h, by epoxy Base silane coupling agent and deionized water are added drop-wise in suspension after mixing, are adjusted pH to 2-3, are stirred with 1000-1500r/min 3-5h is mixed, is centrifuged, filtering is so dry that be alkylated rodlike titanium dioxide granule；It is 1-3wt% acetic acid water that concentration, which is added, in chitosan In solution, be then added and be alkylated rodlike titanium dioxide granule, be stirred to react 30-60min, be centrifuged, filtering, it is dry to get.
Due to chitosan during high temperature cabonization inside micropore be easy to appear contraction the phenomenon that, cause inside chitosan The reduction of adsorption space, this adversely affects the adsorbance of chitosan.The present inventor carries out further for this defect Improvement, processing is modified to chitosan, by silane coupling agent by inorganic rodlike titanium dioxide and organic chitosan It carries out " bridge joint ", after forming chitosan microball, rodlike titanium dioxide plays the role of skeleton, one side energy to chitosan microball The intensity for enough increasing chitosan microball, on the other hand can play the inside supporting role to chitosan microball, in high temperature cabonization Inhibit the contraction of chitosan internal gutter in the process, to help to increase the aperture inside carbonization chitosan, improves chitosan To the adsorption capacity of pernicious gas.
Preferably, the rodlike titanium dioxide granule and the mass ratio of chitosan of being alkylated is 1:5-10.
Preferably, the mass ratio of acrylic resin in the step 2), levelling agent, defoaming agent is 1:0.02-0.05: 0.03-0.06。
Preferably, absorption particle additive amount is the 10-15wt% of acrylic resin in the step 3).
Preferably, the mass ratio of curing agent and acrylic resin is 1:80-90 in the step 4).
Therefore, the invention has the following beneficial effects: the shell cores that (1) absorption particle is coated with silica carbonization chitosan Structure, silica interior have biggish space, can accommodate enough carbonization chitosans, the chitosan microball gap of carbonization Rate is higher, significantly improves pernicious gas adsorption capacity, it is not easy to reach adsorption saturation state；(2) silica shell not only has There is suction-operated that can also form protective effect to the carbonization chitosan of inside cladding；(3) rodlike titanium dioxide is micro- to chitosan Ball plays the role of skeleton, on the one hand can increase the intensity of chitosan microball, on the other hand can play to chitosan microball Inside supporting role, during high temperature cabonization inhibit chitosan internal gutter contraction, thus facilitate increase carbonization shell Chitosan is improved to the adsorption capacity and adsorption efficiency of pernicious gas in aperture inside glycan.
Specific embodiment
Below by specific embodiment, technical scheme is described further.
In the present invention, if not refering in particular to, used raw material and equipment etc. are commercially available or commonly used in the art, Method in embodiment is unless otherwise instructed the conventional method or conventional raw material (analysis is pure) of this field.
Embodiment 1
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g chitosan and 0.8g ammonium chloride is in 2wt% aqueous acetic acid, and stirring and dissolving is added 0.2g emulsifier tween 80 is uniformly mixed to obtain mixed liquor, and 1:2:6 in mass ratio mixes sodium hydroxide, methanol and deionized water Conjunction is configured to condensation water, and mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, and 80mL concentration is added in condensation microballoon and is 3wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 2h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 25:15 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 8g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 7h, centrifuge separation, drying at room temperature obtains silica-chitosan complex microsphere； Silica-chitosan complex microsphere is placed in crucible and is heated to 650 DEG C, calcines 3h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.3g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.5g BYK-141 type defoaming agent stir 1.5h with 400r/min；
3) 1.2g absorption particle is added into the material of step 2), component A is obtained with 100r/min stirring 30min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 2
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g chitosan and 0.8g ammonium chloride is in 3wt% aqueous acetic acid, and stirring and dissolving is added 0.2g emulsifier tween 80 is uniformly mixed to obtain mixed liquor, and 1:2.5:6 in mass ratio is by sodium hydroxide, methanol and deionized water It is hybridly prepared into condensation water, mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, 80mL concentration, which is added, in condensation microballoon is 4wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 2h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 25:20 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 8g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 9h, centrifuge separation, drying at room temperature obtains silica-chitosan complex microsphere； Silica-chitosan complex microsphere is placed in crucible and is heated to 650 DEG C, calcines 3h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.4g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.5g BYK-141 type defoaming agent stir 1h with 500r/min；
3) 1.2g absorption particle is added into the material of step 2), component A is obtained with 200r/min stirring 20min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 3
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g chitosan and 0.6g ammonium chloride is in 1.5wt% aqueous acetic acid, and stirring and dissolving is added 0.2g emulsifier tween 80 is uniformly mixed to obtain mixed liquor, and 1:2:5 in mass ratio mixes sodium hydroxide, methanol and deionized water Conjunction is configured to condensation water, and mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, and 80mL concentration is added in condensation microballoon and is 2wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 1h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 22:10 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 7g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 6h, centrifuge separation, drying at room temperature obtains silica-chitosan complex microsphere； Silica-chitosan complex microsphere is placed in crucible and is heated to 600 DEG C, calcines 5h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.25g BYK-354 type is added in 50wt% aqueous acetone solution Levelling agent and 0.3g BYK-141 type defoaming agent stir 2h with 300r/min；
3) 1g absorption particle is added into the material of step 2), component A is obtained with 100r/min stirring 30min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 4
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g chitosan and 1g ammonium chloride is in 3wt% aqueous acetic acid, and 0.2g is added in stirring and dissolving Emulsifier tween 80 is uniformly mixed to obtain mixed liquor, and 1:3:6 in mass ratio, which mixes sodium hydroxide, methanol and deionized water, to be matched Condensation water is made, mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, it is 5wt% that 80mL concentration, which is added, in condensation microballoon Sodium trimetaphosphate aqueous solution carries out cross-linking reaction 3h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1:30:20 Ammonium hydroxide (analysis is pure), deionized water, ethyl alcohol are mixed, 3g complex microsphere is added in the above-mentioned solution of 100mL, then to mixed liquor Middle dropwise addition 9g tetraethyl orthosilicate, is aged 10h, centrifuge separation, and drying at room temperature obtains silica-chitosan complex microsphere；By two Silica-chitosan compound microsphere, which is placed in crucible, is heated to 650 DEG C, calcines 3h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.5g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.6g BYK-141 type defoaming agent stir 1h with 500r/min；
3) 1.5g absorption particle is added into the material of step 2), component A is obtained with 200r/min stirring 20min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 5
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g chitosan and 0.5g ammonium chloride is in 1wt% aqueous acetic acid, and stirring and dissolving is added 0.2g emulsifier tween 80 is uniformly mixed to obtain mixed liquor, and 1:2:5 in mass ratio mixes sodium hydroxide, methanol and deionized water Conjunction is configured to condensation water, and mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, and 80mL concentration is added in condensation microballoon and is 2wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 1h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 20:10 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 6g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 5h, centrifuge separation, drying at room temperature obtains silica-chitosan complex microsphere； Silica-chitosan complex microsphere is placed in crucible and is heated to 600 DEG C, calcines 5h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.2g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.3g BYK-141 type defoaming agent stir 2h with 300r/min；
3) 1g absorption particle is added into the material of step 2), component A is obtained with 100r/min stirring 30min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 6
The preparation of modification of chitosan:
The rodlike titanium dioxide granule of 5g is dispersed in 120mL dehydrated alcohol, suspension is obtained with 900r/min stirring 2.5h, it will 0.5g KH-560 epoxy silane coupling and 15mL deionized water are added drop-wise in suspension after mixing, adjust pH to 2, 3h is stirred with 1500r/min, is centrifuged, filtering is so dry that be alkylated rodlike titanium dioxide granule；120mL is added in 3g chitosan Concentration is that 1.5g is then added and is alkylated rodlike titanium dioxide granule, is stirred to react 50min in 2wt% aqueous acetic acid, from The heart, filtering, it is dry to get.
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g modification of chitosan and 0.8g ammonium chloride is in 2wt% aqueous acetic acid, and stirring and dissolving adds Enter 0.2g emulsifier tween 80 and be uniformly mixed to obtain mixed liquor, 1:3:6 in mass ratio is by sodium hydroxide, methanol and deionized water It is hybridly prepared into condensation water, mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, 80mL concentration, which is added, in condensation microballoon is 3wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 2h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 25:15 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 8g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 7h, centrifuge separation, drying at room temperature obtains silica-chitosan complex microsphere； Silica-chitosan complex microsphere is placed in crucible and is heated to 600 DEG C, calcines 5h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.3g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.5g BYK-141 type defoaming agent stir 1.5h with 400r/min；
3) 1.2g absorption particle is added into the material of step 2), component A is obtained with 200r/min stirring 20min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 7
The preparation of modification of chitosan:
The rodlike titanium dioxide granule of 5g is dispersed in 150mL dehydrated alcohol, suspension is obtained with 1000r/min stirring 2h, it will 0.5g KH-560 epoxy silane coupling and 20mL deionized water are added drop-wise in suspension after mixing, adjust pH to 3, 3h is stirred with 1500r/min, is centrifuged, filtering is so dry that be alkylated rodlike titanium dioxide granule；150mL is added in 3g chitosan Concentration is that 2g is then added and is alkylated rodlike titanium dioxide granule, is stirred to react 60min, is centrifuged in 3wt% aqueous acetic acid, Filtering, it is dry to get.
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g modification of chitosan and 1g ammonium chloride is in 3wt% aqueous acetic acid, and stirring and dissolving is added 0.2g emulsifier tween 80 is uniformly mixed to obtain mixed liquor, and 1:3:6 in mass ratio mixes sodium hydroxide, methanol and deionized water Conjunction is configured to condensation water, and mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, and 80mL concentration is added in condensation microballoon and is 5wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 3h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 30:20 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 9g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 10h, centrifuge separation, it is compound micro- that drying at room temperature obtains silica-chitosan Ball；Silica-chitosan complex microsphere is placed in crucible and is heated to 650 DEG C, calcines 3h, is cooled to room temperature to obtain absorption Grain；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.5g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.6g BYK-141 type defoaming agent stir 1h with 500r/min；
3) 1.5g absorption particle is added into the material of step 2), component A is obtained with 200r/min stirring 20min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Embodiment 8
The preparation of modification of chitosan:
The rodlike titanium dioxide granule of 5g is dispersed in 100mL dehydrated alcohol, suspension is obtained with 800r/min stirring 3h, by 0.5g KH-560 epoxy silane coupling and 10mL deionized water are added drop-wise in suspension after mixing, adjust pH to 2, with 1000r/min stirs 5h, is centrifuged, filtering, so dry that be alkylated rodlike titanium dioxide granule；It is dense that 100mL is added in 3g chitosan Degree is that 1g is then added and is alkylated rodlike titanium dioxide granule, is stirred to react 30min, is centrifuged, mistake in 1wt% aqueous acetic acid Filter, it is dry to get.
The preparation method of absorbent-type environmental protection coating material, comprising the following steps:
1) 100mL concentration is added in 5g modification of chitosan and 0.5g ammonium chloride is in 1wt% aqueous acetic acid, and stirring and dissolving adds Enter 0.2g emulsifier tween 80 and be uniformly mixed to obtain mixed liquor, 1:2:5 in mass ratio is by sodium hydroxide, methanol and deionized water It is hybridly prepared into condensation water, mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, 80mL concentration, which is added, in condensation microballoon is 2wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 1h, filters, and complex microsphere is dried to obtain in washing at room temperature；By mass ratio 1: 20:10 mixes ammonium hydroxide (analysis pure), deionized water, ethyl alcohol, and 3g complex microsphere is added in the above-mentioned solution of 100mL, then to 6g tetraethyl orthosilicate is added dropwise in mixed liquor, is aged 5h, centrifuge separation, drying at room temperature obtains silica-chitosan complex microsphere； Silica-chitosan complex microsphere is placed in crucible and is heated to 600 DEG C, calcines 5h, is cooled to room temperature to obtain absorption particle；
2) 10g acrylic resin is dissolved in 250mL concentration is that 0.2g BYK-354 type stream is added in 50wt% aqueous acetone solution Flat agent and 0.3g BYK-141 type defoaming agent stir 1h with 500r/min；
3) 1g absorption particle is added into the material of step 2), component A is obtained with 100r/min stirring 30min；
4) 0.5g curing agent is added in 20mL ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
Comparative example 1
The conch meal for not being to replace with the absorption particle in coating equivalent but of comparative example 1 and embodiment 1.
Comparative example 2
Absorption particle in coating the difference from embodiment 1 is that is replaced with the sepiolite of equivalent by comparative example 2.
Experimental test
Adsorption experiment:
Coating is evenly applied on the glass plate having a size of 5cm × 5cm, dry 5h under room temperature；Glass plate is coated with coating On one side upward, it is put into the glass bottom of a cup of 1L, then seal glass cup injects formaldehyde gas into the glass of 1L with syringe Body, the initial concentration for injecting formaldehyde is about D0=3ppm is put into constant incubator and maintains the temperature at 25 DEG C, tests glass afterwards for 24 hours The concentration of formaldehyde is D in glass cup1, calculate the absorptivity m of formaldehyde1；Then the secondary injection formaldehyde gas into glass again, initially Concentration is D0=3ppm tests the concentration D of formaldehyde in glass afterwards for 24 hours2, calculate the absorptivity m of formaldehyde2, m1And m2Calculating it is public Formula is as follows:
m1=(D0-D1)/D0× 100%；
m1=(D0-D2)/D0× 100%；
Embodiment 1 Embodiment 4 Embodiment 5 Embodiment 7 Embodiment 8 Comparative example 1 Comparative example 2
m1(%) 82.5 83.7 80.2 86.5 85.2 68 62
m2(%) 81.6 82.3 80.5 84.4 84.5 35 32
Composite adsorption coating effect prepared by the present invention can be obtained by embodiment and comparative example comparison and be much better than common absorption coating； Compared by embodiment 4 and embodiment 7 available, the effect of paint-absorbable formaldehyde of the chitosan Jing Guo modified preparation is better than shell Glycan does not pass through modified coating, this is because rodlike titanium dioxide plays the inside supporting role to chitosan microball, in height Inhibit the contraction of chitosan internal gutter in warm carbonisation, to help to increase the aperture inside carbonization chitosan, improves Adsorption capacity and adsorption efficiency of the chitosan to pernicious gas.
The adsorption rate and a formaldehyde adsorption of available second adsorption formaldehyde of the present invention are compared by secondary formaldehyde absorbing Absorptivity it is suitable, less, and the absorptivity of second adsorption formaldehyde is greatly reduced relative to primary absorption in comparative example, says for variation The absorption of adsorbent PARA FORMALDEHYDE PRILLS(91,95) starts to tend to saturation state in bright comparative example.
Performance measurement:
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, although this Invention has been disclosed in a preferred embodiment above, and however, it is not intended to limit the invention, any person skilled in the art, It does not depart within the scope of technical solution of the present invention, when the technology contents using the disclosure above make a little change or are modified to equivalent The equivalent embodiment of variation, but without departing from the technical solutions of the present invention, according to the technical essence of the invention to the above reality Any simple modification, equivalent change and modification made by example are applied, all of which are still within the scope of the technical scheme of the invention.

Claims (8)

1. a kind of preparation method of absorbent-type environmental protection coating material, which comprises the following steps:
1) concentration is added in chitosan and ammonium chloride is in 1-3wt% aqueous acetic acid, and emulsifier tween 80 is added in stirring and dissolving It is uniformly mixed to obtain mixed liquor, mixed liquor is added drop-wise in condensation water, obtains condensation microballoon, it is 2- that concentration, which is added, in condensation microballoon 5wt% sodium trimetaphosphate aqueous solution carries out cross-linking reaction 1-3h, filters, and complex microsphere is dried to obtain in washing at room temperature；By ammonium hydroxide, go Ionized water and ethyl alcohol mix to obtain mixed liquor, and complex microsphere is added, and tetraethyl orthosilicate is then added dropwise into mixed liquor, are aged 5- 10h, centrifuge separation, drying at room temperature obtain silica-chitosan complex microsphere；Silica-chitosan complex microsphere is placed in It is heated to 600-650 DEG C in crucible, calcines 3-5h, is cooled to room temperature to obtain absorption particle；
2) acrylic resin is dissolved in aqueous acetone solution, levelling agent and defoaming agent is added, 1- is stirred with 300-500r/min 2h；
3) absorption particle is added into the material of step 2, component A is obtained with 100-200r/min stirring 20-30min；
4) curing agent is added in ethyl acetate and is uniformly mixed to obtain B component；
5) absorbent-type environmental protection coating material is stirred evenly to obtain after mixing component A with B component.
2. a kind of preparation method of absorbent-type environmental protection coating material according to claim 1, which is characterized in that in the step 1) The mass ratio of chitosan and ammonium chloride is 1:0.1-0.2.
3. a kind of preparation method of absorbent-type environmental protection coating material according to claim 1, which is characterized in that in the step 1) Condensation water includes sodium hydroxide, methanol and deionized water；The mass ratio of the three is 1:2-3:5-6.
4. a kind of preparation method of absorbent-type environmental protection coating material according to claim 1, which is characterized in that in the step 1) The mass ratio of complex microsphere and tetraethyl orthosilicate is 1:2-3.
5. a kind of preparation method of absorbent-type environmental protection coating material according to claim 1, which is characterized in that in the step 1) Chitosan into cross modification, method of modifying the following steps are included:
Rodlike titanium dioxide granule is dispersed in dehydrated alcohol, suspension is obtained with 800-1000r/min stirring 2-3h, by epoxy Base silane coupling agent and deionized water are added drop-wise in suspension after mixing, are adjusted pH to 2-3, are stirred with 1000-1500r/min 3-5h is mixed, is centrifuged, filtering is so dry that be alkylated rodlike titanium dioxide granule；It is 1-3wt% acetic acid water that concentration, which is added, in chitosan In solution, be then added and be alkylated rodlike titanium dioxide granule, be stirred to react 30-60min, be centrifuged, filtering, it is dry to get.
6. a kind of preparation method of absorbent-type environmental protection coating material according to claim 5, which is characterized in that the alkylation stick The mass ratio of shape titanium dioxide granule and chitosan is 1:5-10.
7. a kind of preparation method of absorbent-type environmental protection coating material according to claim 1, which is characterized in that in the step 2 Acrylic resin, levelling agent, defoaming agent mass ratio be 1:0.02-0.05:0.03-0.06.
8. a kind of preparation method of absorbent-type environmental protection coating material according to claim 1, which is characterized in that in the step 3) Adsorb the 10-15wt% that particle additive amount is acrylic resin.
CN201910637459.5A 2019-07-15 2019-07-15 A kind of preparation method of absorbent-type environmental protection coating material Withdrawn CN110204972A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116854104A (en) * 2023-07-31 2023-10-10 同济大学 Binder-free molecular sieve particle material, preparation method and micro-speaker

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108434122A (en) * 2018-05-23 2018-08-24 华中科技大学 Polyelectrolyte hydridization hollow silica nanoparticles and the preparation method and application thereof
CN109266196A (en) * 2018-09-17 2019-01-25 湘江涂料科技有限公司 A kind of high solid acrylic polyurethane finish paint and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108434122A (en) * 2018-05-23 2018-08-24 华中科技大学 Polyelectrolyte hydridization hollow silica nanoparticles and the preparation method and application thereof
CN109266196A (en) * 2018-09-17 2019-01-25 湘江涂料科技有限公司 A kind of high solid acrylic polyurethane finish paint and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116854104A (en) * 2023-07-31 2023-10-10 同济大学 Binder-free molecular sieve particle material, preparation method and micro-speaker

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Application publication date: 20190906