CN112409822A - 一种水性涂料专用纳米碳酸钙的制备方法 - Google Patents
一种水性涂料专用纳米碳酸钙的制备方法 Download PDFInfo
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 74
- 239000003973 paint Substances 0.000 title claims abstract description 41
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 9
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 9
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 9
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 7
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 7
- 229930006000 Sucrose Natural products 0.000 claims abstract description 7
- 238000003763 carbonization Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 7
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 7
- 239000005720 sucrose Substances 0.000 claims abstract description 7
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 239000011575 calcium Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 150000003385 sodium Chemical class 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 230000005587 bubbling Effects 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 20
- 239000004408 titanium dioxide Substances 0.000 abstract description 10
- 238000001556 precipitation Methods 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000004062 sedimentation Methods 0.000 abstract description 3
- 239000012767 functional filler Substances 0.000 abstract description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 239000011734 sodium Substances 0.000 abstract 1
- 229910052708 sodium Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 229940077386 sodium benzenesulfonate Drugs 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
本发明一种水性涂料专用纳米碳酸钙的制备方法，采用三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的混合物为晶型控制剂，松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的混合物为改性剂，通过碳化、表面改性和解聚，制得水性涂料专用纳米碳酸钙，其堆积密度达到0.40g/cm3以下、白度为98%以上，沉降体积70ml/g以上。作为功能填料应用于水性涂料中，本发明纳米碳酸钙抗沉淀能力强，分散性好,具有很好的悬浮性和储存稳定性，在水性涂料中的添加量大，能部分替代昂贵的钛白粉，降低产品成本，并赋予涂膜高遮盖力、附着力，光泽度高，流平性好。
Description
所属领域
本发明涉及一种水性涂料专用纳米碳酸钙的制备方法，具体属于纳米碳酸钙制备技术领域。
背景技术
碳酸钙、二氧化钛和立德粉是涂料常用的填料。二氧化钛的白度高，遮盖力强，是一种重要的白色颜料，但密度较大，一般为3.7～4.3 g/cm3，在涂料胶液中易沉降，使用成本高。立德粉遮盖力较强，密度同样也大，一般为4.1～4.3 g/cm3，其折射率和不透明性仅次于二氧化钛，使用成本也较高。水性涂料对光泽度、流变性和耐久性的要求，需要碳酸钙更多赋予功能化。碳酸钙具有空间位阻效应，在水性涂料中，能使水性涂料配方中密度较大的立德粉和钛白粉悬浮，起到防沉降的作用，可以部分取代钛白粉和其它颜料，使水性涂料具有良好的开罐效果，降低了水性涂料的成本。一般的碳酸钙颗粒粒径较大，同样存在易沉淀，亲水性差等不足，难以有效替代水性涂料中的钛白粉和立德粉等材料，而双亲改性后的纳米碳酸钙具有亲水、亲油的特点，在水性涂料中有良好的分散性，而且能够改善钛白粉等填料在水性涂料中的抗沉淀性，使水性涂料胶体体系更加稳定。双亲改性纳米碳酸钙的堆积密度较小，一般为0.4%~0.6g/ cm3，白度一般为96%-97%，密度仍然偏大，抗沉淀能力还有待提高。
发明内容
本发明针对水性涂料的现状，提出一种水性涂料专用纳米碳酸钙的制备方法，通过颗粒粒径控制和双亲改性, 使纳米碳酸钙具有强的抗沉淀能力，且白度高和分散性好，应用于水性涂料中, 具有良好的悬浮性和储存稳定性。
本发明一种水性涂料专用纳米碳酸钙的制备方法采用三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的混合物为晶型控制剂，松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的混合物为改性剂，通过碳化、表面改性和解聚，制得水性涂料专用纳米碳酸钙，具体过程为：
将精制Ca(OH)2浆料陈化18-24h，再经振动筛和旋液分离器6级除渣，调节其质量浓度至10%~20%、温度至20~35℃后，加入Ca(OH)2质量的0.3%～1.5％的晶型控制剂，搅拌混合均匀，之后通入体积浓度为20%～40%的CO2气体进行鼓泡碳化反应，直到浆料pH为6.5～7碳化终点，得到质量浓度为10%～20％的熟浆；将熟浆除渣后，边搅拌边升温，温度到达65~85℃后加入Ca(OH)2质量的2%～8％的改性剂，调节pH值为7～9，搅拌改性60～90min；得到改性的纳米碳酸钙悬浊液经压滤脱水、烘干解聚，制得水性涂料专用纳米碳酸钙；
所述的松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的质量比依次为1∶2∶1；晶型控制剂三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的质量比依次为1∶2∶1∶1。
所述的调节pH的试剂为硫酸锌、硫酸铝、氯化钙、磷酸或乙酸。
本发明的有益效果：
本发明一种水性涂料专用纳米碳酸钙的制备方法通过颗粒粒径控制和双亲改性, 制备的纳米碳酸钙堆积密度达到0.40g/cm3以下、白度为98%以上，沉降体积70ml/g以上。作为功能填料应用于水性涂料中,纳米碳酸钙抗沉淀能力强，分散性好, 具有很好的悬浮性和储存稳定性，在水性涂料中的添加量大，能部分替代昂贵的钛白粉,降低产品成本，并同时赋予涂膜高遮盖力和附着力，光泽度高，流平性好。
具体实施方式
实施例1
水性涂料专用纳米碳酸钙的制备过程为：
将精制Ca(OH)2浆料陈化20h，再经过6级除渣，调节其质量浓度至12%、温度至25℃后，加入Ca(OH)2质量的1.0％的晶型控制剂，搅拌混合均匀，之后通入体积浓度为30%的CO2气体进行鼓泡碳化反应，直到反应体系pH为7，得到质量浓度为12％的熟浆；将熟浆除渣后，边搅拌边升温，温度到达75℃后加入Ca(OH)2质量的5%的改性剂，调节pH值为7，搅拌改性80min；得到改性的纳米碳酸钙悬浊液经压滤脱水、烘干解聚，制得堆积密度达到0.38g/cm3的水性涂料专用纳米碳酸钙。其中：晶型控制剂三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的质量比为1∶2∶1∶1；改性剂松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的质量比依次为1∶2∶1。
实施例2
一种水性涂料专用纳米碳酸钙的制备方法，其特征在于：所述的制备方法具体过程为：
将精制Ca(OH)2浆料陈化18h，再次经过三级除渣，调节其质量浓度至10%、温度至20℃后，加入Ca(OH)2质量的1.5％的晶型控制剂，搅拌混合均匀，之后通入体积浓度为25%的CO2气体进行鼓泡碳化反应，直到反应体系pH为6.5，得到质量浓度为10%％的熟浆；将熟浆除渣后，边搅拌边升温，温度到达80℃后加入Ca(OH)2质量的4％的改性剂，调节pH值为7，搅拌改性90min；得到改性的纳米碳酸钙悬浊液经压滤脱水、烘干解聚，制得堆积密度达到0.35g/cm3的水性涂料专用纳米碳酸钙。
其中：晶型控制剂三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的质量比为1∶2∶1∶1；改性剂松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的质量比依次为1∶2∶1。
实施例3
制备水性聚氨酯涂料：
水性聚氨酯230克、堆积密度0.35g/cm3的水性涂料专用纳米碳酸钙10克经高速分散均匀后，再加入堆积密度0.35g/cm3的水性涂料专用纳米碳酸钙70克、钛白粉30克、去离子水60克、3克分散剂KYC9366、2克流平剂DL-80、3克消泡剂980F、乙二醇5克和苯磺酸钠3克，在2000rmp的转速下高速分散后，得到A组分；以水性聚氨酯固化剂S-2和脱芳烃环保溶剂-08型作为B组分；A组分和B组分按照质量比为2∶1的量复配使用。制备的水性涂料固体含量高，水性胶体稳定，不易沉淀，漆膜丰满坚韧，并可与乳胶漆等其他油漆同时施工，漆膜具有高光，高附着力和高柔韧性等优点。
Claims (2)
1.一种水性涂料专用纳米碳酸钙的制备方法，其特征在于：所述的制备方法采用三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的混合物为晶型控制剂，松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的混合物为改性剂，通过碳化、表面改性和解聚，制得水性涂料专用纳米碳酸钙，具体过程为：
将精制Ca(OH)2浆料陈化18-24h，再经振动筛和旋液分离器6级除渣，调节其质量浓度至10%~20%、温度至20~35℃后，加入Ca(OH)2质量的0.3%～1.5％的晶型控制剂，搅拌混合均匀，之后通入体积浓度为20%～40%的CO2气体进行鼓泡碳化反应，直到浆料pH为6.5～7碳化终点，得到质量浓度为10%～20％的熟浆；将熟浆除渣后，边搅拌边升温，温度到达65~85℃后加入Ca(OH)2质量的2%～8％的改性剂，调节pH值为7～9，搅拌改性60～90min；得到改性的纳米碳酸钙悬浊液经压滤脱水、烘干解聚，制得水性涂料专用纳米碳酸钙；
所述的改性剂松香基三季铵盐、苯基三乙氧基硅烷和聚乙二醇的质量比依次为1∶2∶1；晶型控制剂三聚磷酸钠、二聚酸钠、硫酸锌和蔗糖的质量比依次为1∶2∶1∶1。
2.根据权利要求1所述的一种水性涂料专用纳米碳酸钙的制备方法，其特征在于：所述的调节pH的试剂为硫酸锌、硫酸铝、氯化钙、磷酸或乙酸。
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