CN1065440A - 溶液诱发浓酸制白炭黑 - Google Patents
溶液诱发浓酸制白炭黑 Download PDFInfo
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- CN1065440A CN1065440A CN 91102200 CN91102200A CN1065440A CN 1065440 A CN1065440 A CN 1065440A CN 91102200 CN91102200 CN 91102200 CN 91102200 A CN91102200 A CN 91102200A CN 1065440 A CN1065440 A CN 1065440A
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- carbon black
- white carbon
- water glass
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000006229 carbon black Substances 0.000 title claims abstract description 20
- 239000002253 acid Substances 0.000 title description 9
- 238000000034 method Methods 0.000 claims abstract description 17
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000012452 mother liquor Substances 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 9
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000007171 acid catalysis Methods 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 235000019241 carbon black Nutrition 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Glass Compositions (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Silicon Compounds (AREA)
Abstract
本发明提供了一种生产白炭黑的方法,使用浓硫
酸和催化液,在一定的温度和pH值条件下中和水玻
璃得到性能优异的白炭黑。本方法可以实现反应条
件的优化控制,节省原料,简化生产工艺,缩短反应时
间,减少设备和管路的腐蚀和污染问题。产品白度
好、粒径小,比表面积大,pH值为6.7~7.5,假密度
0.18~0.21g/cm3,真密度2g/cm3,SiO2含量
>90%,游离水含量≤6%,折射率1.45~1.46,吸油
值2.4~2.7ml/g。
Description
本发明提供了一种用浓硫酸催化中和水玻璃制橡胶补强剂、造纸填料、油漆消光剂等多种用途白炭黑的方法。
沉淀法是以稀酸中和水玻璃或硅酸钠溶液生产白炭黑的一种方法。(见GB2,169,129A;SU326,847)。该法需配制稀酸溶液,使用氯化钠或硫酸钠作分散剂。随着酸的不断加入,PH值由12逐渐减小到8左右。因此,在这个过程中,始终都有白炭黑沉淀生成,降低了产品性能,延长了反应时间,一般需3小时左右。要制得性能优异的白炭黑,还需要选择下列方法中的一种进行处理:(1).加有机溶剂后经临界压力法或恒沸蒸馏法;(2).冷冻干燥法;(3).加极性溶剂和非极性溶剂常规处理后,再高温活化。
为了改进这种生产方法存在操作步骤多、耗费原材料、输送稀酸腐蚀管路和设备、废水不符合排放标准等弊病。发明了溶液诱发浓酸制白炭黑的方法。
本发明用白炭黑的母液为催化液,予热后,将浓硫酸和含SiO2的水玻璃计量加入进行中和反应,其反应式为:
其中:m代表水玻璃的模数
n代表结合水的分子数
这样,确保白炭黑始终在PH为7~9时析出。水玻璃的加入量是母液体积的0.6~1.0倍,在此情况下可以保证产品的性能,反应时间也缩到原来的50%,然后,升温保持一段时间,再加浓硫酸,使反应液的PH值继续降至2~4。中和反应结束,过滤(母液备用),用热水洗涤产品,干燥,包装。
整个工艺比较简单。用此方法制得白炭黑的技术指标为:
外观:白色松散粉状物;
SiO2含量:>90%;
水含量:≤6%;
假密度:0.18~0.21克/厘米3;
PH值(100%悬浊液):6.7~7.5;
灼烧失重(950℃,2小时):≤9%;
吸油值:2.4~2.7毫升/克;
粒径:7~100nm;
钠离子含量:≤1%;
Fe2O3含量:≤0.1%;
比表面积:≥250米2/克;
细度:200目筛余物0%;
折射率:1.45~1.46;
真密度:2克/厘米3;
本发明提供的浓硫酸诱发溶液中和水玻璃制白炭黑,由于使用了浓硫酸,而不是配制稀酸溶液,按常规处理后,不必再采用冷冻干燥法,临界压力法或恒沸蒸馏法及高温活化处理,从而减化了操作步骤,减少了设备和管路的腐蚀。中和反应是利用了前次制备白炭黑的母液为催化液,因而具有特殊的功效,不需要再加分散剂,这样就节省了原材,缩短了制备工艺的生产周期。也由于母液已被利用,洗涤液的PH值在6以上,就可以达到国家规定的排放标准,克服了稀酸中和法所带来的许多缺点。
实施例
将白炭黑的母液作为催化液,予热到20~60℃,在搅拌下,加入含SiO2浓度为8~20%水玻璃,使溶液的PH值为7~9,升温到不超过70℃,再同时计量加入上述浓度的水玻璃和浓硫酸,保持溶液的PH值不变。水玻璃加入量是母液体积的0.6~1.0倍,时间为20分钟,调节PH值为7~10,升温至70~100℃,保持40分钟。然后,再加浓硫酸,使溶液的PH值为2~5,停止加热,10分钟后进行过滤,滤出的母液备用。
再用整个反应溶液体积1.2倍的80~100℃净水洗涤滤并,送喷雾干燥器干燥,成品装袋。
Claims (3)
1、一种用浓酸催化法中和水玻璃制白炭黑的方法,其特征在于使用每次生产白炭黑的母液作为催化液,将含有SiO2的水玻璃加入到催化液中,用浓硫酸在搅拌下,PH值保持在7~10范围内,中和制得性能优异的白炭黑。
2、按权利要求1所述的方法,其特征在于催化液需要予热到20~60℃,在搅拌下,再加入8~20%SiO2的水玻璃,用83~98%浓硫酸中和来制备白炭黑。
3、按权利要求1、2所述的方法,其特征在于中和制白炭黑时,同时计量加入83~98%浓硫酸和8~20%SiO2的水玻璃,保持溶液的PH值不变。然后调节PH值在7~10,在70~100℃,保持40分钟。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 91102200 CN1065440A (zh) | 1991-04-03 | 1991-04-03 | 溶液诱发浓酸制白炭黑 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 91102200 CN1065440A (zh) | 1991-04-03 | 1991-04-03 | 溶液诱发浓酸制白炭黑 |
Publications (1)
Publication Number | Publication Date |
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CN1065440A true CN1065440A (zh) | 1992-10-21 |
Family
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Family Applications (1)
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CN 91102200 Pending CN1065440A (zh) | 1991-04-03 | 1991-04-03 | 溶液诱发浓酸制白炭黑 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1039219C (zh) * | 1993-12-21 | 1998-07-22 | 冯中一 | 一种雾化法生产水合硅酸的方法 |
CN102602946A (zh) * | 2012-03-21 | 2012-07-25 | 陈君华 | 循环利用含有硫酸钠的废水制备高比表面白炭黑的方法 |
CN103466644A (zh) * | 2013-09-07 | 2013-12-25 | 安徽确成硅化学有限公司 | 一种疏水性白炭黑的制备方法 |
CN103466643A (zh) * | 2013-08-21 | 2013-12-25 | 安徽确成硅化学有限公司 | 一种母液循环利用的制备白炭黑的方法 |
-
1991
- 1991-04-03 CN CN 91102200 patent/CN1065440A/zh active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1039219C (zh) * | 1993-12-21 | 1998-07-22 | 冯中一 | 一种雾化法生产水合硅酸的方法 |
CN102602946A (zh) * | 2012-03-21 | 2012-07-25 | 陈君华 | 循环利用含有硫酸钠的废水制备高比表面白炭黑的方法 |
CN102602946B (zh) * | 2012-03-21 | 2022-04-08 | 安徽科技学院 | 循环利用含有硫酸钠的废水制备高比表面白炭黑的方法 |
CN103466643A (zh) * | 2013-08-21 | 2013-12-25 | 安徽确成硅化学有限公司 | 一种母液循环利用的制备白炭黑的方法 |
CN103466644A (zh) * | 2013-09-07 | 2013-12-25 | 安徽确成硅化学有限公司 | 一种疏水性白炭黑的制备方法 |
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