CN116715265A - 一种超细BaSO4/TiO2复合材料的制备方法 - Google Patents
一种超细BaSO4/TiO2复合材料的制备方法 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 229910010413 TiO 2 Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 50
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003607 modifier Substances 0.000 claims abstract description 12
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000011734 sodium Substances 0.000 claims description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 12
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 11
- 235000011152 sodium sulphate Nutrition 0.000 claims description 11
- 238000009826 distribution Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 7
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- JMGZBMRVDHKMKB-UHFFFAOYSA-L disodium;2-sulfobutanedioate Chemical compound [Na+].[Na+].OS(=O)(=O)C(C([O-])=O)CC([O-])=O JMGZBMRVDHKMKB-UHFFFAOYSA-L 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 229930182470 glycoside Natural products 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 125000003563 glycoside group Chemical group 0.000 claims 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical class [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 abstract description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 11
- 239000004094 surface-active agent Substances 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 6
- 239000004408 titanium dioxide Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- -1 glucoside citrate Chemical class 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 229930182478 glucoside Natural products 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- CJDPJFRMHVXWPT-UHFFFAOYSA-N barium sulfide Chemical compound [S-2].[Ba+2] CJDPJFRMHVXWPT-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 150000002338 glycosides Chemical group 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- C01F11/46—Sulfates
- C01F11/462—Sulfates of Sr or Ba
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
本发明属于硫酸钡化合物领域，具体涉及一种超细BaSO4/TiO2复合材料的制备方法。该方法包括：步骤1：在碳酸钡浆料中加入复合改性剂，再加入Na2SO4溶液，超声反应；步骤2：加入硫酸氧钛，继续超声反应，过滤、洗涤、干燥，即得超细BaSO4/TiO2复合材料。本发明利用硫酸氧钛水解产生二氧化钛直接包覆到经过复合表面活性剂改性的超细硫酸钡粒子上，工艺简单，资源循环利用，经济环保无废物产生，同时能达到对超细硫酸钡大小及性能的有效控制，适宜于产业化生产应用。
Description
技术领域
本发明属于硫酸钡化合物领域，具体涉及一种超细BaSO4/TiO2复合材料的制备方法。
背景技术
硫酸钡因其具有白度高、化学性稳定性高、资源丰富、价格低廉等优点而被广泛地应用于涂料、油墨、橡胶、医药、塑料、纺织，钻探等领域。近年来，随着应用领域对产品不断升级，普通硫酸钡由于粉体颗粒粒度大，分布不均、表面性能单一，杂质含量较高，批次之间差异性大等已不能满足产品需要。人们设法开发一些满足市场要求的超细功能性硫酸钡制备技术，建立高附加值的硫酸钡微粉生产线，继而来提高我国硫酸钡的市场竞争力。
专利文献CN106976900B公开了采用经过焙烧还原成硫化钡的重晶石与已除去钙镁等杂质的芒硝溶液反应制取硫酸钡，并通过表面修饰及分散剂硬脂酸钠对新生的硫酸钡晶核进行表面修饰，采用表面改性剂高分子聚合物对硫酸钡颗粒进行进一步的表面修饰，使其能与粉末涂料中的有机高分子进行有效的结合并在涂料中很好地分散。该方法制备的硫酸钡用于生产的粉末涂料具有高白度、流平性好、分散均匀等优点。专利文献CN103881418B公开了以硫酸钡浆料为原料，添加润滑剂、改性剂、分散剂、偶联剂、热稳定剂、抗氧剂等制备出了粒径为10-1000nm的硫酸钡粒子。专利文献CN101418140B公开了将碳酸钡、硫酸溶液和隔离剂进行合成反应，反应后得到的硫酸钡粉体悬浮液经熟化、分离、洗涤、浆化后再进行表面改性处理，干燥后得到成品。但上述技术工艺路线程复杂，设备投资高，不易于产业化生产。因此，亟待开发一种工艺简单且易于产业化应用的超细功能性硫酸钡制备技术。
发明内容
为解决上述现有技术中存在的技术问题，本发明提供一种工艺简单、资源循环利用、对环境无污染、易于产业化应用的表面活性剂改性的超细BaSO4/TiO2复合材料的制备方法。
为实现上述目的，本发明是通过以下技术方案来实现：
一种超细BaSO4/TiO2复合材料的制备方法，包括以下步骤：
步骤1：在碳酸钡浆料中加入复合改性剂，再加入Na2SO4溶液，超声反应；
步骤2：加入硫酸氧钛，继续超声反应，过滤、洗涤、干燥，即得超细BaSO4/TiO2复合材料。
所述方法的制备反应式如下：
BaCO3 + Na2SO4 ＝ BaSO4 + Na2CO3 (1)
TiOSO4 + H2O ＝ TiO2 + H2SO4 (2)
BaCO3 + H2SO4＝ BaSO4 +H2O+CO2 (3)
Na2CO3 + H2SO4＝ Na2SO4 +H2O+CO2 (4)
作为优选，在所述步骤1中，碳酸钡浆料的质量浓度为30％。
作为优选，在所述步骤1中，复合改性剂为糖苷柠檬酸酯APG-EC和窄分布脂肪醇聚氧乙烯醚AEO9、单烷基二甲基羟乙基氯化铵或窄分布AEO9磺基琥珀酸酯二钠盐按照质量比1:1～1:3复配得到的复合表面改性剂。
作为优选，在所述步骤1中，复合改性剂的添加量为碳酸钡含量的1‰～5‰。
作为优选，在所述步骤1中，碳酸钡和硫酸钠的摩尔比为1:1～1:1.5。
作为优选，在所述步骤1中，Na2SO4溶液的质量浓度为20％～40％。
作为优选，在所述步骤1中，超声反应的功率为1000W～2000W，反应温度为30℃～50℃，反应时间为2h-8h。
作为优选，在所述步骤2中，硫酸氧钛的物质的量为碳酸钡物质的量的0.05-0.5倍。
作为优选，在所述步骤2中，超声反应的功率为500-1000w功率，反应温度为30℃～50℃，反应时间为0.5h～1h。
作为优选，在所述步骤2中，超细BaSO4/TiO2复合材料的粒子粒径为100nm～300nm，白度为95％～98％，比表面积为20～50g/cm2。
与现有技术相比，本发明的有益效果如下：
本发明采用无机二氧化钛对超细硫酸钡粒子进行包覆，同时添加复合表面活性剂对超细BaSO4/TiO2复合材料进行改性，一方面利用二氧化钛白度高的特点，可以解决硫酸钡作为颜料白度低的问题，另一方面利用二氧化钛比表面积大的特点，改善超细硫酸钡比表面积小的不足，改善在应用过程中填加量小的不足。
本发明利用硫酸氧钛水解产生二氧化钛直接包覆到经过复合表面活性剂改性的超细硫酸钡粒子上，产生的副产物硫酸可以将未反应的碳酸钡转化为硫酸钡，提高了反应转化率，同时又与副产物碳酸钠反应生成硫酸钠，硫酸钠又可作为生成硫酸钡的反应原料，这样就达到了资源的循环利用。此外，在制备过程中所添加的改性剂复合表面活性剂有效地控制了超细BaSO4/TiO2复合材料粒径分布不均匀及团聚现象，进而有效地调控以单分散状态下的小粒径集中分布情况。同时在制备过程中通过超声波的空化作用，可以有效地提高由碳酸钡向硫酸钡的转化速率。该方法工艺简单，资源循环利用，经济环保无废物产生，同时能达到对超细BaSO4/TiO2大小及性能的有效控制，适宜于产业化生产应用。
具体实施方式
为了便于理解本发明，下面将对本发明进行更全面的描述。但是，本发明可以以许多不同的形式来实现，并不限于本文所描述的实施例。相反地，提供这些实施例的目的是使对本发明的公开内容的理解更加透彻全面。
实施例1
称取60g碳酸钡加入140ml蒸馏水中配制成30％的浆料，并加入0.3g(5‰)复合表面活性剂(由糖苷柠檬酸酯(APG-EC)和窄分布脂肪醇聚氧乙烯醚AEO9按照质量比1:1复配得到)，再加入20％浓度的Na2SO4溶液，碳酸钡和硫酸钠的摩尔比为1:1，在超声功率为1000W超声波作用下，于30℃，反应2h；然后直接加入相对于碳酸钡物质的量0.05倍的硫酸氧钛，继续以500w功率超声反应0.5h，过滤液浓缩Na2SO4回收率达85％，可用于反应原料硫酸钠循环利用，产物经过滤、洗涤、110℃干燥，即得超细BaSO4/TiO2复合材料，其粒子粒径100nm±10nm，白度Wr为95.5％，比表面积SBET为50g/cm2。
实施例2
称取60g碳酸钡加入140ml蒸馏水中配制成30％的浆料，并加入0.6g复合表面活性剂(由糖苷柠檬酸酯(APG-EC)和单烷基二甲基羟乙基氯化铵按照质量比1:2复配得到)，再加入40％浓度的Na2SO4溶液，碳酸钡和硫酸钠的摩尔比为1:1.5，在超声功率为2000w超声波作用下，于50℃，反应8h；然后直接加入相对于碳酸钡物质的量0.5倍的硫酸氧钛，继续以1000w功率超声反应1h，过滤液浓缩Na2SO4回收率达90％，可用于反应原料硫酸钠循环利用，产物经过滤、洗涤、110℃干燥，即得超细BaSO4/TiO2复合材料，其粒子粒径为300nm±20nm，白度Wr为96％，比表面积SBET为30g/cm2。
实施例3
称取60g碳酸钡加入140ml蒸馏水中配制成30％的浆料，并加入0.4g复合表面活性剂(由糖苷柠檬酸酯(APG-EC)和窄分布脂肪醇聚氧乙烯醚AEO9按照质量比1:3复配得到)，再加入30％浓度的Na2SO4溶液，碳酸钡和硫酸钠的摩尔比为1:1.4，在超声功率为1500W超声波作用下，于40℃，反应6h；然后直接加入相对于碳酸钡物质的量0.1倍的硫酸氧钛，继续以800w功率超声反应1h，过滤液浓缩Na2SO4回收率达90％，可用于反应原料硫酸钠循环利用，产物经过滤、洗涤、110℃干燥，即得超细BaSO4/TiO2复合材料，其粒子粒径为150nm±10nm，白度Wr为97％，比表面积SBET为48g/cm2。
实施例4
称取60g碳酸钡加入140ml蒸馏水中配制成30％的浆料，并加入0.5g复合表面活性剂(由糖苷柠檬酸酯(APG-EC)和窄分布AEO9磺基琥珀酸酯二钠盐按照质量比1:2复配得到)，再加入35％浓度的Na2SO4溶液，碳酸钡和硫酸钠的摩尔比为1:1.2，在超声功率为2000w超声波作用下，于50℃，反应7h；然后直接加入相对于碳酸钡物质的量0.3倍的硫酸氧钛，继续以1000w功率超声反应0.8h，过滤液浓缩Na2SO4回收率达92％，可用于反应原料硫酸钠循环利用。产物经过滤、洗涤、110℃干燥，即得超细BaSO4/TiO2复合材料，其粒子粒径为200nm±10nm，白度Wr为98％，比表面积SBET为40g/cm2。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (10)
1.一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，包括以下步骤：
步骤1：在碳酸钡浆料中加入复合改性剂，再加入Na2SO4溶液，超声反应；
步骤2：加入硫酸氧钛，继续超声反应，过滤、洗涤、干燥，即得超细BaSO4/TiO2复合材料。
2.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤1中，碳酸钡浆料的质量浓度为30％。
3.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤1中，复合改性剂为糖苷柠檬酸酯APG-EC和窄分布脂肪醇聚氧乙烯醚AEO9、单烷基二甲基羟乙基氯化铵或窄分布AEO9磺基琥珀酸酯二钠盐按照质量比1:1～1:3复配得到的复合表面改性剂。
4.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤1中，复合改性剂的添加量为碳酸钡含量的5‰～1％。
5.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤1中，碳酸钡和硫酸钠的摩尔比为1:1～1:1.5。
6.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤1中，Na2SO4溶液的质量浓度为20％～40％。
7.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤1中，超声反应的功率为1000W～2000W，反应温度为30℃～50℃，反应时间为2h-8h。
8.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤2中，硫酸氧钛的物质的量为碳酸钡物质的量的0.05-0.5倍。
9.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤2中，超声反应的功率为500-1000w功率，反应温度为30℃～50℃，反应时间为0.5h～1h。
10.根据权利要求1所述的一种超细BaSO4/TiO2复合材料的制备方法，其特征在于，在所述步骤2中，超细BaSO4/TiO2复合材料的粒子粒径为100nm～300nm，白度为95％～98％，比表面积为20～50g/cm2。
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