CN100497411C - Aqueous wood lacquer emulsions and wood lacquer of the same - Google Patents

Abstract

The invention provides a preparation method of waterborne woodenware finishes emulsion and the waterborne woodenware finishes emulsion prepared by the method. The method is that a nano TiO2 sizing agent is added during the synthetic process of the emulsion and comprises the following raw materials of the weight portion ratio: TiO2: 1.5 to 4; surfactant: 0.04 to 0.08; water: 3 to 6. The invention adopts the nano TiO2 sizing agent to participate in the polyreaction of the emulsion to make the nano TiO2 sizing agent distribute evenly in the emulsion and not move during drying the paint film, therefore, the waterborne woodenware finishes prepared by the emulsion not only has good stability, that is, precipitate will not happen even if stored over 6 months, but also has good resistance to temperature fluctuations, phototropy resistance and antibacterial property.

Description

A kind of aqueous wood lacquer latex and wood lacquer thereof

Technical field

The present invention relates to a kind of aqueous wood lacquer latex and aqueous woodware paint thereof, particularly the ACRYLIC EMULSION of aqueous woodware paint, aqueous woodware paint prepared therefrom and preparation method thereof.

Background technology

Wood lacquer in the market is still oil-base paint mostly, but oil-base paint exists and pollutes and to problems such as the demand of organic solvent are big.Compare with the oiliness wood lacquer, the characteristics that it is nonpoisonous and tasteless, pollution-free that aqueous woodware paint has etc., therefore in today that environmental issue receives much attention, the development of aqueous woodware paint and maturation be a kind of certainty trend.

The existing common preparation method of aqueous woodware paint is: adopt in the adding mixing kettles such as aqueous wood lacquer latex, deionized water, auxiliary agent, mill base, after stirring again thickening make.What the aqueous woodware paint paint film was had the greatest impact is the performance of emulsion, because there are very big difference in the membrane formation mechanism of water-based emulsion and oil-base paint, therefore the performance behind the emulsion film forming is also generally not as oil-base paint, exist paint film soft partially, in the problem prior aries such as wear resistance and fast light discolouration difference, for aqueous woodware paint is carried out modification, normally in the paint process, add the nano pulp for preparing, nanoparticle and emulsion particle in this nanometer waterborne woodware lacquer do not form bonding action preferably, though can tentatively strengthen filming of aqueous woodware paint, can make the compactness of filming, performances such as water tolerance are significantly improved, but, the nanometer waterborne woodware lacquer that obtains in this method is stored unstable, and nano particle moves in film process, reunite, cause problem such as skewness in filming, make that some performances of nanometer waterborne woodware lacquer are not well embodied, therefore never obtain excellent popularization.

At present, modal aqueous wood lacquer latex has two kinds of the aqueous polyurethane emulsions of the ACRYLIC EMULSION of single-component and two components on the market.The ACRYLIC EMULSION paint film is softer, but ageing resistance is good; The polyaminoester emulsion of two components need now add solidifying agent when using, inconvenience during use, and ageing-resistant performance is relatively poor, easy xanthochromia etc.The somebody is composite water soluble acrylic acid and urethane, but can not fundamentally address the above problem.

Publication number is to disclose a kind of woodenware use polyaminoester emulsion in the Chinese patent application of CN1827690, this method prepares the initial latex of aqueous polyurethane emulsion by the polyester glycol that makes with aromatic diacid acid anhydride and aliphatic diacid and glycol mixing copolymerization, utilize polyacrylic ester to improve the water tolerance of aqueous polyurethane again, thereby make woodenware use polyaminoester emulsion, this polyurethane aqueous wood lacquer emulsion is the composite emulsion of a kind of typical acroleic acid polyurethane, has above-mentioned problem.

Summary of the invention

The objective of the invention is the problem that exists at above prior art and a kind of fast light variable color aqueous wood lacquer latex, aqueous woodware paint and preparation method thereof are provided, the emulsifying stage for preparing at this wood lacquer emulsion has added the nano-TiO that is used for modification ₂Slurry makes its polyreaction that participates in emulsion, thereby forms nano-TiO ₂The heterozygosis aqueous wood lacquer latex has good fast light variable color and germ resistance with the aqueous woodware paint of this emulsion preparation.

Be to realize that the object of the invention, one aspect of the present invention provide a kind of preparation method of aqueous wood lacquer latex and by the aqueous wood lacquer latex of this method preparation, this method is included in the emulsion process of raw material and adds nano-TiO ₂Slurry.

Nano-TiO wherein ₂Slurry comprises following raw materials in weight portion: TiO ₂: 1.5-4; Tensio-active agent: 0.04-0.08; Water: 3-6.

The opposing party's purpose of the present invention provides a kind of preparation method of aqueous wood lacquer latex and the aqueous wood lacquer latex that is prepared by this method, and this method comprises following step of carrying out in turn:

1) get the raw materials ready according to following weight part proportioning:

Methyl methacrylate 40-85; Diacetone-acryloamide(DAA) 1-7; Butyl acrylate 15-55; Emulsifying agent 1.0-2.0; Sodium lauryl sulphate 1.0-2.0; Initiator 0.4-1.0; Sodium bicarbonate 0.3-0.6; PH regulator agent 1.0-2.5; Defoamer 0.3-0.8; Deionized water 70-100; Nano-TiO ₂Slurry 4-10;

2) in reactor, add first deionized water 30-50 weight part, emulsifying agent 0.1-0.3 weight part and sodium lauryl sulphate 0.1-0.3 weight part, stir and intensification;

When 3) being warming up to 75 ± 5 ℃, add first initiator solution, add-on is the 25-40% of initiator total amount;

4) whole methyl methacrylates, whole butyl acrylates, whole diacetone-acryloamide(DAA)s are mixed evenly, then to the emulsifying agent that adds surplus, the sodium lauryl sulphate of surplus, whole sodium bicarbonates, second batch of initiator, balance of deionized water and whole nano-TiOs ₂Drip in the mixing kettle of oxide slurry, carry out emulsification, second crowd of 40-50% that initiator is the initiator total amount wherein dripped behind all material reemulsification 40-80 minutes, formed pre-emulsion;

5) in reactor, drip pre-emulsion, drip off in 2-4 hour;

6) after reaction under 80 ± 2 ℃, add the initiator of surplus, be warming up to 85-90 ℃, be incubated 1.5-2.5 hour;

7) add whole defoamer and pH regulator agent, stir, adjust pH 7-8 is cooled to below 40 ℃ discharging.

Wherein, emulsifying agent select alkylphenol polyoxyethylene and or alkylphenol polyoxyethylene ammonium sulfate; Initiator select ammonium persulphate and or Potassium Persulphate; One or more in ammoniacal liquor, trolamine and the 2-amino-2-methyl-1-propanol are selected in the pH regulator agent; Defoamer is selected silicone based or metallic soap defoamer.

Particularly, nano-TiO wherein ₂Slurry is mixed by following raw materials in weight portion: TiO ₂: 1.5-4; Tensio-active agent: 0.04-0.08; Water: 3-6.

Particularly, tensio-active agent is the compound of sodium polyacrylate or polyacrylamide and nonionogenic tenside.

Particularly, described nano-TiO ₂Oxide slurry prepares by following steps:

1) nano-TiO ₂, water, surfactant-dispersed form slurry, again slurry is ground;

2) slurry after grinding was applied the ultrasonic wave effect 2-4 hour at least.

Another object of the present invention provides a kind of aqueous woodware paint and preparation method thereof, and this method may further comprise the steps:

1) get the raw materials ready according to following weight part proportioning:

Nano-TiO ₂Oxide compound emulsion 70-90, water-based wax emulsion 3-6, film coalescence aid 3-6, wetting agent 0.2-0.5, butyl glycol ether 0.5-1.5, thickening material 0.1-0.5, defoamer 0.1-0.3, deionized water 3-8;

2) deionized water is added in the paint mixing tank, then film coalescence aid, wetting agent, butyl glycol ether, thickening material and defoamer are added in the paint mixing tank successively, stir;

3) add nano-TiO ₂Oxide compound emulsion and water-based wax emulsion, after stirring, discharging.

Nano-TiO wherein ₂The oxide compound emulsion is made according to the method described above.

Wherein, film coalescence aid is selected 12 carbon alcohol esters; Wetting agent is selected polyether-modified polysiloxane-based; Thickening material is selected polyamine class or polyureas thickening material; Defoamer is selected silicone based or metallic soap defoamer.

Aqueous wood lacquer latex and aqueous woodware paint by the present invention's preparation have the following advantages:

Emulsion of the present invention is owing to add the composite nano oxide (Al of modification in the emulsifying stage of preparation process ₂O ₃And TiO ₂) slurry, make its polyreaction that participates in emulsion, thereby nano material being evenly distributed in emulsion, can not move in the dried coating film process, aqueous woodware paint stability prepared therefrom significantly strengthens, and stores and can not precipitate more than 6 months.

In addition, not only have stronger fast light discoloration by the aqueous woodware paint of emulsion preparation of the present invention, and have good antimicrobial property.

Embodiment

Describe content of the present invention in detail below by specific embodiment.

Embodiment 1

(1) aqueous wood lacquer latex preparation

Produce aqueous wood lacquer latex according to following steps:

1, get the raw materials ready according to following weight proportion:

Methyl methacrylate (MMA) 50kg

Diacetone-acryloamide(DAA) (DAAM) 5kg

Butyl acrylate (BA) 45kg

Alkylphenol polyethoxye ether ammonium sulfate (R-436) 1.6kg

Sodium lauryl sulphate (SDS) 1.5kg

Nano-TiO ₂Slurry 5kg

Sodium bicarbonate (SBC) 0.4kg

Potassium Persulphate (KSP) 0.5kg

Deionized water (H ₂O) 100kg

Trolamine 1.8kg

Defoamer (BYK-028) 0.5kg

Nano-TiO wherein ₂Slurry prepares according to following steps:

1) get the raw materials ready according to following weight part proportioning:

Nano-TiO ₂: 3; Tensio-active agent sodium polyacrylate: 0.05; Water: 5;

Tensio-active agent also can be selected the mixture of aniorfic surfactant or anion surfactant and nonionogenic tenside, except that sodium polyacrylate, also can select the mixture of polyacrylamide, sodium polyacrylate or polyacrylamide and nonionogenic tenside (as PO-EO block compound or polyoxyethylene nonylphenol ether).

2) prepare nano-TiO by mechanical milling method ₂Oxide slurry is nano-TiO ₂Oxide compound, water, tensio-active agent are dispersed into slurry in dispersion machine, wherein temperature is controlled to be 25 ℃; Slurry is joined in the sand mill again and ground 3 hours, controlled temperature is 25 ℃; Be prepared into nano-TiO ₂Oxide slurry;

3) with step 2) nano-TiO that obtains ₂Oxide slurry under the ultrasonic wave condition between 4 hours after, discharging;

2, in the reactor that agitator, prolong, nitrogen protection and feeding device are housed, add alkylphenol polyethoxye ether ammonium sulfate (R-436) and the 0.3kg sodium lauryl sulphate (SDS) of 50kg deionized water and 0.3kg, be stirred to each component and mix;

When 3, making reactor be warming up to 75 ℃, add the Potassium Persulphate (KSP) of 0.2kg;

4,50kg methyl methacrylate (MMA), 45kg butyl acrylate (BA), 5kg diacetone-acryloamide(DAA) (DAAM) are mixed evenly, then to adding 1.3kg alkylphenol polyethoxye ether ammonium sulfate (R-436), 1.2kg sodium lauryl sulphate (SDS), 0.4kg sodium bicarbonate (SBC), 0.2kg Potassium Persulphate (KSP), 50kg deionized water and 5kg nano-TiO ₂Drip methyl methacrylate, butyl acrylate and diacetone-acryloamide(DAA) miscellany in the mixing kettle of slurry in 2 hours, carry out pre-emulsification, reemulsification is 60 minutes after reinforced the finishing, and gets pre-emulsion;

5, in reactor, drip the pre-emulsion of preparation in the step 4, in 4 hours, drip off;

6, keep 80 ± 2 ℃ temperature of reaction after 2 hours, add the 0.1kg Potassium Persulphate (KSP) of surplus, be warming up to 85-90 ℃, be incubated 2 hours;

7, add 0.5Kg defoamer and 1.8Kg trolamine, stir, be cooled to below 40 ℃ discharging.

The performance index of the product emulsion that is obtained are as follows

Solids content 47%

Emulsion particle diameter 200nm

PH value 7.5

Viscosity (25 ± 0.5 ℃) 300mpa.s

Zhu Cun Qi ≧ 6 months

(2) aqueous woodware paint preparation

Produce aqueous woodware paint according to following steps:

1, get the raw materials ready according to following weight proportion:

Film coalescence aid (12 carbon alcohol ester) 3kg

Wetting agent (BYK-346) 0.1kg

Butyl glycol ether 0.8kg

Deionized water 5.0kg

Thickening material (PU-85) 0.1kg

Defoamer (BYK-028) 0.1kg

The embodiment of the invention 1 emulsion 80kg

Water-based wax emulsion 5.0kg

2,5.0kg distilled water is put into paint mixing tank, then 3kg film coalescence aid alcohol ester 12,0.1kg wetting agent, 0.8kg butyl glycol ether, 0.1kg thickening material, 0.1kg defoamer are added paint mixing tank, stir simultaneously;

3, add 80kg emulsion of the present invention and 5.0kg water-based wax emulsion, stir discharging.

The performance index of the aqueous woodware paint product that is obtained are as follows:

Solids content 42%

Viscosity (25 ± 0.5 ℃) 800mpa.s

Zhu Cun Qi ≧ 6 months

Embodiment 2:

(1) aqueous wood lacquer latex

Produce aqueous wood lacquer latex according to following steps:

1, get the raw materials ready according to following weight proportion:

Methyl methacrylate (MMA) 72kg

Diacetone-acryloamide(DAA) (DAAM) 3kg

Butyl acrylate (BA) 25kg

Alkylphenol polyethoxy ether (OP-10) 1.7kg

Sodium lauryl sulphate (SDS) 1.7kg

Nano-TiO ₂Slurry 8kg

Sodium bicarbonate (SBC) 0.3kg

Potassium Persulphate (KSP) 0.6kg

Deionized water (H ₂O) 95kg

Ammoniacal liquor (NH ₃H ₂O) 2kg

Defoamer (NXZ) 0.3kg

Nano-TiO wherein ₂Slurry prepares according to following steps:

1) get the raw materials ready according to following weight part proportioning:

Nano-TiO ₂: 4; Tensio-active agent polyacrylamide: 0.08; Water: 6;

2) prepare nano-TiO by mechanical milling method ₂Oxide slurry is nano-TiO ₂Oxide compound, water, tensio-active agent are dispersed into slurry in dispersion machine, wherein temperature is controlled to be 25 ℃; Slurry is joined in the sand mill again and ground 3 hours, controlled temperature is 25 ℃; Be prepared into nano-TiO ₂Oxide slurry;

3) with step 2) nano-TiO that obtains ₂Oxide slurry under the ultrasonic wave condition between ultrasonic 4 hours after, discharging;

2, in the reactor that agitator, prolong, nitrogen protection and feeding device are housed, add alkylphenol polyethoxy ether (OP-10) and the 0.2kg sodium lauryl sulphate (SDS) of 50kg deionized water and 0.2kg, be stirred to each component and mix;

When 3, making reactor be warming up to 75 ℃, add the Potassium Persulphate (KSP) of 0.2kg;

4,72kg methyl methacrylate (MMA), 25kg butyl acrylate (BA), 3kg diacetone-acryloamide(DAA) (DAAM) are mixed evenly, then to adding 1.5kg alkylphenol polyethoxy ether (OP-10), 1.5kg sodium lauryl sulphate (SDS), 0.3kg sodium bicarbonate (SBC), 0.3kg Potassium Persulphate (KSP), 45kg deionized water and 8kg nano-TiO ₂Drip methyl methacrylate, butyl acrylate and diacetone-acryloamide(DAA) miscellany in the mixing kettle of slurry in 2 hours, carry out pre-emulsification, reemulsification is 60 minutes after reinforced the finishing;

5, in reactor, drip the pre-emulsion of preparation in the step 4, in 3 hours, drip off;

6, keep 80 ± 2 ℃ temperature of reaction after 2 hours, add the 0.1kg Potassium Persulphate (KSP) of surplus, be warming up to 85-90 ℃, be incubated 2 hours;

7, add 0.3Kg defoamer and 2Kg ammoniacal liquor and stir, be cooled to below 40 ℃ discharging.

The performance index of the product emulsion that is obtained are as follows

Solids content 48%

Emulsion particle diameter 200nm

PH value 7.5

Viscosity (25 ± 0.5 ℃) 300mpa.s

Zhu Cun Qi ≧ 6 months

(2) aqueous woodware paint

Produce aqueous woodware paint according to following steps:

1, get the raw materials ready according to following weight proportion:

Film coalescence aid (12 carbon alcohol ester) 4kg

Wetting agent (BYK-346) 0.2kg

Butyl glycol ether 1.0kg

Deionized water 6.0kg

Thickening material (BYK-410) 0.2kg

Defoamer (NXZ) 0.2kg

The embodiment of the invention 2 emulsion 83kg

Water-based wax emulsion 4.0kg

2, the 6.0kg deionized water is put into paint mixing tank, then 4kg film coalescence aid, 0.2kg wetting agent, 1.0kg butyl glycol ether, 0.2kg thickening material, 0.2kg defoamer are added paint mixing tank, stir simultaneously;

3, add 83kg emulsion of the present invention and 4.0kg water-based wax emulsion, stir discharging.

The performance index of the aqueous woodware paint product that is obtained are as follows:

Solids content 40%

Viscosity (25 ± 0.5 ℃) 10 00mpa.s

Zhu Cun Qi ≧ 6 months

Embodiment 3:

(1) aqueous wood lacquer latex

Produce aqueous wood lacquer latex according to following steps:

1, get the raw materials ready according to following weight proportion:

Methyl methacrylate (MMA) 60kg

Diacetone-acryloamide(DAA) (DAAM) 5kg

Butyl acrylate (BA) 35kg

Alkylphenol polyethoxye ether ammonium sulfate (R-436) 1.5kg

Sodium lauryl sulphate (SDS) 1.4kg

Nano-TiO ₂Slurry 6kg

Sodium bicarbonate (SBC) 0.5kg

Ammonium persulphate (APS) 0.4kg

Deionized water (H ₂O) 90kg

2-amino-2-methyl-1-propanol (AMP-95) 1.5kg

Defoamer (NXZ) 0.4kg

Nano-TiO wherein ₂Slurry prepares according to following steps:

1) get the raw materials ready according to following weight part proportioning:

Nano-TiO ₂: 2; Tensio-active agent: 0.04; Water: 4;

Wherein, tensio-active agent is the compound of sodium polyacrylate and PO-EO block compound.

2) prepare nano-TiO by mechanical milling method ₂Oxide slurry is nano-TiO ₂Oxide compound, water, tensio-active agent are dispersed into slurry in dispersion machine, wherein temperature is controlled to be 25 ℃; Slurry is joined in the sand mill again and ground 3 hours, controlled temperature is 25 ℃; Be prepared into nano-TiO ₂Oxide slurry;

3) with step 2) nano-TiO that obtains ₂Oxide slurry under the ultrasonic wave condition between ultrasonic 4 hours after, discharging;

2, in the reactor that agitator, prolong, nitrogen protection and feeding device are housed, add alkylphenol polyethoxye ether ammonium sulfate (R-436) and the 0.1kg sodium lauryl sulphate (SDS) of 30kg deionized water and 0.1kg, be stirred to each component and mix;

When 3, making reactor be warming up to 75 ℃, add the ammonium persulphate (APS) of 0.1kg;

4,60kg gram methyl methacrylate (MMA), 35kg butyl acrylate (BA), 5kg diacetone-acryloamide(DAA) (DAAM) are mixed evenly, then to adding 1.4kg alkylphenol polyethoxye ether ammonium sulfate, 1.3kg sodium lauryl sulphate (SDS), 0.5kg sodium bicarbonate (SBC), 0.2kg ammonium persulphate (APS), 60kg deionized water and 6kg nano-TiO ₂Drip methyl methacrylate, butyl acrylate and diacetone-acryloamide(DAA) miscellany in the mixing kettle of slurry in 2 hours, carry out pre-emulsification, reemulsification is 60 minutes after reinforced the finishing;

5, in reactor, drip the pre-emulsion of preparation in the step 4, in 2 hours, drip off;

6, keep 80 ± 2 ℃ temperature of reaction after 2 hours, add the 0.1kg ammonium persulphate (APS) of surplus, be warming up to 85-90 ℃, be incubated 2 hours;

7, add 0.4Kg defoamer and 1.5Kg AMP-95, stir, be cooled to below 40 ℃ discharging.

The performance index of the product emulsion that is obtained are as follows

Solids content 50%

Emulsion particle diameter 200nm

PH value 7.5

Viscosity (25 ± 0.5 ℃) 300mpa.s

Zhu Cun Qi ≧ 6 months

(2) aqueous woodware paint

Produce aqueous woodware paint according to following steps:

1, get the raw materials ready according to following weight proportion:

Film coalescence aid (12 carbon alcohol ester) 5kg

Wetting agent (Wet-500) 0.2kg

Butyl glycol ether 1.1kg

Deionized water 8.0kg

Thickening material (BYK-410) 0.3kg

Defoamer (BYK-028) 0.2kg

The embodiment of the invention 3 emulsion 85kg

Water-based wax emulsion 5.0kg

2, the 8.0kg deionized water is put into paint mixing tank, then 5kg film coalescence aid, 0.2kg wetting agent, 1.1kg butyl glycol ether, 0.3kg thickening material, 0.2kg defoamer are added paint mixing tank, stir simultaneously.

3, add 85kg emulsion of the present invention and 5.0kg water-based wax emulsion, stir discharging.

The performance index of the aqueous woodware paint product that is obtained are as follows:

Solids content 43%

Viscosity (25 ± 0.5 ℃) 1100mpa.s

Zhu Cun Qi ≧ 6 months

Embodiment 4:

(1) aqueous wood lacquer latex

Produce aqueous wood lacquer latex according to following steps:

1, get the raw materials ready according to following weight proportion:

Methyl methacrylate (MMA) 65kg

Diacetone-acryloamide(DAA) (DAAM) 3kg

Butyl acrylate (BA) 32kg

Alkylphenol polyethoxy ether (OP-10) 1.7kg

Sodium lauryl sulphate (SDS) 1.7kg

Nano-TiO ₂Slurry 4kg

Sodium bicarbonate (SBC) 0.6kg

Ammonium persulphate (APS) 0.5kg

Deionized water (H ₂O) 100kg

Trolamine 2.5kg

Defoamer (BYK-028) 0.5kg

Nano-TiO wherein ₂Slurry prepares according to following steps:

1) get the raw materials ready according to following weight part proportioning:

Nano-TiO ₂: 1.5; Tensio-active agent: 0.04; Water: 3;

Wherein, tensio-active agent is the compound of polyacrylamide and polyoxyethylene nonylphenol ether.

2) prepare nano-TiO by mechanical milling method ₂Oxide slurry is nano-TiO ₂Oxide compound, water, tensio-active agent are dispersed into slurry in dispersion machine, wherein temperature is controlled to be 25 ℃; Slurry is joined in the sand mill again and ground 3 hours, controlled temperature is 25 ℃; Be prepared into nano-TiO ₂Oxide slurry;

3) with step 2) nano-TiO that obtains ₂Oxide slurry under the ultrasonic wave condition between ultrasonic 4 hours after, discharging;

2, in the reactor that agitator, prolong, nitrogen protection and feeding device are housed, add alkylphenol polyethoxy ether (OP-10) and the 0.3kg sodium lauryl sulphate (SDS) of 50kg deionized water and 0.3kg, be stirred to each component and mix;

When 3, making reactor be warming up to 75 ℃, add the ammonium persulphate (APS) of 0.2kg;

4,65kg methyl methacrylate (MMA), 32kg butyl acrylate (BA), 3kg diacetone-acryloamide(DAA) (DAAM) are mixed evenly, then to adding 1.4kg alkylphenol polyethoxye ether ammonium sulfate (R-436), 1.4kg sodium lauryl sulphate (SDS), 0.6kg sodium bicarbonate (SBC), 0.2kg ammonium persulphate (APS), 50kg deionized water and 4kg nano-TiO ₂Drip methyl methacrylate, butyl acrylate and diacetone-acryloamide(DAA) miscellany in the mixing kettle of slurry in 2 hours, carry out pre-emulsification, reemulsification is 60 minutes after reinforced the finishing;

5, in reactor, drip the pre-emulsion of preparation in the step 4, in 4 hours, drip off;

6, keep 80 ± 2 ℃ temperature of reaction after 2 hours, add the 0.1kg ammonium persulphate (APS) of surplus, be warming up to 85-90 ℃, be incubated 2 hours;

7, add 0.5kg defoamer (BYK-028) and 2.5kg trolamine and stir, be cooled to below 40 ℃ discharging.

The performance index of the product emulsion that is obtained are as follows:

Solids content 47%

Emulsion particle diameter 200nm

PH value 7.5

Viscosity (25 ± 0.5 ℃) 300mpa.s

Zhu Cun Qi ≧ 6 months

(2) aqueous woodware paint

Produce aqueous woodware paint according to following steps:

1, get the raw materials ready according to following weight proportion:

Film coalescence aid (12 carbon alcohol ester) 4kg

Wetting agent (Wet-500) 0.2kg

Butyl glycol ether 0.9kg

Deionized water 6.0kg

Thickening material (PU-85) 0.2kg

Defoamer (NXZ) 0.2kg

The embodiment of the invention 4 emulsion 84kg

Water-based wax emulsion 4.0kg

2, the 6.0kg deionized water is put into paint mixing tank, then 4kg film coalescence aid, 0.2kg wetting agent, 0.9kg butyl glycol ether, 0.2kg thickening material, 0.2kg defoamer are added paint mixing tank, stir;

3, add 84kg emulsion of the present invention and 4.0kg water-based wax emulsion, stir discharging.

The performance index of the aqueous woodware paint product that is obtained are as follows:

Solids content 41%

Viscosity (25 ± 0.5 ℃) 1000mpa.s

Zhu Cun Qi ≧ 6 months

Reference examples one

Adopt self-control emulsion preparation aqueous woodware paint, the compound method of emulsion is not except that adding composite nano-oxide slurry, and all the other steps are identical with the embodiment of the invention 1, and the preparation process of aqueous woodware paint is identical with embodiment 1.

Reference examples two

Adopt self-control emulsion preparation aqueous woodware paint, the compound method of emulsion is not except that adding composite nano-oxide slurry, and all the other steps are identical with the embodiment of the invention 2, and the preparation process of aqueous woodware paint is identical with embodiment 2

Reference examples three

Adopt self-control emulsion preparation aqueous woodware paint, the compound method of emulsion is not except that adding composite nano-oxide slurry, and all the other steps are identical with the embodiment of the invention 3, and the preparation process of aqueous woodware paint is identical with embodiment 3.

Reference examples four

Adopt self-control emulsion preparation aqueous woodware paint, the compound method of emulsion is not except that adding composite nano-oxide slurry, and all the other steps are identical with the embodiment of the invention 4, and the preparation process of aqueous woodware paint is identical with embodiment 4

Press the GB3186 regulation to the aqueous woodware paint sampling, again by national standard " the general preparation method of paint film (GB-T1727-1992) " working method, preparation paint film test specimen.Use paint film spreader (80 μ m) to be coated with by the film thickness specified requirement, contain calculating admittedly by 45%, theoretical build is 36 μ m.The paint film of preparation is placed a dry week under the condition of fixed temperature and humidity lucifuge.Be positioned over cool place, dry storage.

Experimental example one fast light discoloration test

(Xenon Fade Meter, X25F Japan) detect the phototropic that dyes the bright red colored single palte test specimen of 0.5% acid GR to adopt xenon optical attenuation instrument.

Concrete experimental technique is: accelerated deterioration under certain light intensity, temperature and humidity; (CR-300MINOLTA Japan) measures the aberration of colored single palte, and with CIE (1976) L with the Minolta colour-difference meter ^*, a ^*, b ^*Colour system table look calculates the total color difference Δ E*ab of illumination front and back, is the variable color degree of different light time.

Xenon rayed test conditions: illumination 42w/m ², temperature 50-60 ℃, humidity 60%.

Model is placed on the specimen mounting in the xenon optical attenuation instrument, carry out (h) illumination in 100 hours after, with the Minolta colour-difference meter test plate (panel) is carried out wood color and measures, note brightness value L, colourimetric number a and b, and calculate total color difference by following formula:

Luminosity equation: $\mathrm{\ΔL}*={L*}_1-{L*}_2$

Colour difference: $\mathrm{\Δa}*={a*}_1-{a*}_2$ ? $\mathrm{\Δb}*={b*}_1-{b*}_2$

Total color difference: ${{\mathrm{\ΔE}}^{*}}_{\mathrm{ab}}=\sqrt{{\left({\mathrm{\ΔL}}^{*}\right)}^2+{\left({\mathrm{\Δa}}^{*}\right)}^2+{\left({\mathrm{\Δb}}^{*}\right)}^2}$

Wherein 1 expression does not apply the time point of illumination as yet, behind the 2 expression illumination 100h.

The calculation result of total color difference sees Table 1 after 100 hours

Variable color controlled trial result that table 1 is fast light

Test specimen	Total color difference
		Embodiment 1	10.823093
Embodiment 2	9.969731
		Embodiment 3	11.560282
Embodiment 4	12.950075
		Reference examples 1	27.810698
Reference examples 2	25.417047
		Reference examples 3	25.504481
Reference examples 4	26.268469

As seen from Table 1, compare aqueous woodware paint, colored single palte is had the effect of obvious suppression phototropic with the aqueous woodware paint of the emulsion preparation of embodiment of the invention 1-4 with the reference examples emulsion preparation.

Experimental example two antibacterial tests

Detect according to Nippon Standard " antibiotic fabricated product-antibacterial activity test method and antibacterial effect (JIS Z 2801:2000) " for nanometer waterborne woodware lacquer paint film germ resistance, this standard is that the antibacterial effect on antibiotic fabricated product (comprising intermediate) surface is estimated.Use two kinds of bacterium of gram yin, yang respectively: streptococcus aureus (staphylococcus aurous) and intestinal bacteria (Escherichia coli) detect, than the more comprehensive anti-microbial property that shows body surface.Antibacterial tests the results are shown in Table 2

Table 2 nano-TiO ₂The antibacterial tests of aqueous wooden ware paint film and common aqueous woodware paint film

As seen from Table 2, compare aqueous woodware paint, have apparent bacteriostatic action with the aqueous woodware paint of the emulsion preparation of embodiment of the invention 1-4 with the reference examples emulsion preparation.

Claims (6)

1, a kind of preparation method of emulsion of aqueous woodware paint is characterized in that comprising following step of carrying out in turn:

1) get the raw materials ready according to following weight part proportioning:

Methyl methacrylate 40-85; Diacetone-acryloamide(DAA) 1-7; Butyl acrylate 15-55; Emulsifying agent 1.0-2.0; Sodium lauryl sulphate 1.0-2.0; Initiator 0.4-1.0; Sodium bicarbonate 0.3-0.6; PH regulator agent 1.0-2.5; Defoamer 0.3-0.8; Deionized water 70-100; Nano-TiO ₂Slurry 4-10; Wherein, described emulsifying agent select alkylphenol polyoxyethylene and or alkylphenol polyoxyethylene ammonium sulfate; Described nano-TiO ₂Slurry is mixed by following raw materials in weight portion: nano-TiO ₂: 1.5-4; Tensio-active agent: 0.04-0.08; Water: 3-6;

2) in reactor, add first deionized water 30-50 weight part, emulsifying agent 0.1-0.3 weight part and sodium lauryl sulphate 0.1-0.3 weight part, stir and intensification;

When 3) being warming up to 75 ± 5 ℃, add first initiator, add-on is the 25-40% of initiator total amount;

4) whole methyl methacrylates, whole butyl acrylates, whole diacetone-acryloamide(DAA)s are mixed evenly, then to the emulsifying agent that adds surplus, the sodium lauryl sulphate of surplus, whole sodium bicarbonates, second batch of initiator, balance of deionized water and whole nano-TiOs ₂Drip methyl methacrylate, butyl acrylate and diacetone-acryloamide(DAA) miscellany in the mixing kettle of slurry, carry out emulsification, second crowd of 40-50% that initiator is the initiator total amount wherein dripped behind all material reemulsification 40-80 minutes, formed pre-emulsion;

5) in reactor, drip pre-emulsion;

6) after reacting under 80 ± 2 ℃ the temperature, add the initiator of surplus, be warming up to 85-90 ℃, be incubated 1.5-2.5 hour;

7) add whole defoamer and pH regulator agent, stir, the pH value is transferred to 7-8, be cooled to below 40 ℃ discharging.

2, the method for claim 1 is characterized in that: described initiator select ammonium persulphate and or Potassium Persulphate; One or more in ammoniacal liquor, trolamine and the 2-amino-2-methyl-1-propanol are selected in described pH regulator agent; Described defoamer is selected silicone based or metallic soap defoamer.

3, the preparation method of emulsion as claimed in claim 1 is characterized in that: described nano-TiO ₂The preparation process of slurry comprises:

1) nano-TiO ₂, water, tensio-active agent mixes and is dispersed into slurry, again slurry is ground;

2) after the product that grinds being applied between ultrasonic wave effect 4 hours, discharging.

4,, it is characterized in that the compound of described tensio-active agent selection aniorfic surfactant or anion surfactant and nonionogenic tenside as the preparation method of the arbitrary described emulsion of claim 1-3.

5, a kind of emulsion of aqueous woodware paint is characterized in that being prepared from according to the arbitrary described method of claim 1-3.

6, a kind of aqueous woodware paint is characterized in that containing according to the described emulsion of claim 5.