CN1073463A - 红色有机-无机包核颜料 - Google Patents
红色有机-无机包核颜料 Download PDFInfo
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- CN1073463A CN1073463A CN 91111775 CN91111775A CN1073463A CN 1073463 A CN1073463 A CN 1073463A CN 91111775 CN91111775 CN 91111775 CN 91111775 A CN91111775 A CN 91111775A CN 1073463 A CN1073463 A CN 1073463A
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- component solution
- solution
- coupling component
- inorganic pigment
- pigment extender
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- 239000000049 pigment Substances 0.000 title claims abstract description 15
- 238000005859 coupling reaction Methods 0.000 claims abstract description 30
- 230000008878 coupling Effects 0.000 claims abstract description 21
- 238000010168 coupling process Methods 0.000 claims abstract description 21
- 239000004606 Fillers/Extenders Substances 0.000 claims abstract description 12
- 239000001023 inorganic pigment Substances 0.000 claims abstract description 12
- 125000000664 diazo group Chemical group [N-]=[N+]=[*] 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 6
- 239000008399 tap water Substances 0.000 claims description 4
- 235000020679 tap water Nutrition 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 240000004160 Capsicum annuum Species 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 235000010288 sodium nitrite Nutrition 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims description 2
- 239000010813 municipal solid waste Substances 0.000 claims description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 2
- 229910052731 fluorine Inorganic materials 0.000 claims 2
- 239000011737 fluorine Substances 0.000 claims 2
- 239000000243 solution Substances 0.000 description 17
- 239000000463 material Substances 0.000 description 8
- 230000006911 nucleation Effects 0.000 description 8
- 238000010899 nucleation Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 230000000176 photostabilization Effects 0.000 description 5
- 239000012954 diazonium Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-O diazynium Chemical compound [NH+]#N IJGRMHOSHXDMSA-UHFFFAOYSA-O 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000006193 diazotization reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920002681 hypalon Polymers 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3063—Treatment with low-molecular organic compounds
-
- C—CHEMISTRY; METALLURGY
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
本发明属于有机包核颜料的制造方法。本发明
是将重氮组分溶液加入到含有无机体质颜料的偶合
组分溶液中，进行偶合反应，然后过滤、洗涤、干燥、粉
碎，得到有机-无机包核颜料。
Description
本发明属于有机包核颜料的制造方法。
红色有机-无机包核颜料（以下称包核大红粉），是有机包核颜料的一种，它以廉价白色颜料或天然矿物微粒为核心，外层以大红粉包复，再进行无机包膜处理而成。
关于有机包核颜料，国外从六十年代，国内从七十年代即已开始研究。研究的重点侧重于核的选择，助剂的配伍，合成工艺等方面，而具体到包核大红粉的详细报导至今尚未见报导。国内市场曾出现过一种“88复合大红粉”，严格地说，这不是一种包核颜料，而是一种混拼型颜料，它的着色力、耐光性等指标都很差。八十年代后期，由于颜料中间体价格猛涨，货源短缺，致使大红粉价格持续上涨，涂料行业为此承受更大的负担。因此，找到一种价格较低、性能与大红粉相当的产品，成为涂料行业的强烈要求。
针对以上情况，本发明的目的在于，采用合成的方法，以廉价的白色无机体质颜料为核心，通过偶合反应，使大红粉颗粒紧密地包复在核的外层，构成真正的红色有机-无机包核颜料，即包核大红粉。
本发明采用超细无机体质颜料为核心，将其加入到合成大红粉的偶合组份溶液中去，然后再将重氮组份加入到含有成核材料的偶合组份溶液中去，在偶合反应过程中使生成的大红粉颗粒包复在核体上，经保温、过滤、洗涤、干燥和粉碎等工序得到成品。
制备纯有机大红粉，已有比较成熟的技术，是将重氮组份与偶合组份进行偶合反应而制得。
制备重氮组份是将29.30g的苯胺加入到100ml水中，再加入1+1的盐酸130～140ml，搅拌成均匀液体，配制成盐酸苯胺溶液，加入碎冰冷却至0℃左右。然后在搅拌条件下，滴加27%的亚硝酸钠溶液进行重氮化反应，温度控制在0～5℃，反应后期滴加速度减慢。用新制备的碘化钾淀粉试纸测定反应终点，即得到重氮组份溶液。
偶合组份是将30～40ml，40%的氢氧化钠溶液和15～20g的红油溶于250～300ml水中，加热至90℃左右，加入84g色酚AS，搅拌使之完全溶解，然后加水稀释，得到体积为1200～1500ml偶合组份溶液。
本发明以0.5∶1的比例将无机体质颜料加入到偶合组份溶液中去并搅拌均匀。成核材料的选择十分重要，因它们的性质将直接影响包核颜料的性质。可以做为成核材料的无机体质颜料很多，有超细二氧化硅、活性白土、超细膨润土、高岭土、沉淀碳酸钡以及超细滑石粉等。本发明采用超细无机体质颜料为成核材料，粒度分布在1～5μ，加入比例为0.5～1.0。
在搅拌状态下，将重氮组份溶液，慢慢地加入到含有成核材料的偶合溶液中，二者的体积比为1∶2，进行偶合反应，控制偶合反应温度30～60℃，重氮液的加入速度为20～60ml/min，反应时间为10～30分钟，终点PH值控制在8～12。反应完成后，进行保温、过滤、洗涤、干燥、粉碎得到产品。
充分实施本发明，可以得到以超细无机体质颜料为核心，色泽纯正的红色有机-无机包核颜料，其吸油值在35～50范围，着色力（与有机大红粉比较）在75～85范围，水溶物10%以下。使用本发明生产的包核大红粉，在大红醇酸磁漆、氯磺化聚乙烯漆中使用，可以代替100%的大红粉，生产成本将会得到显著降低。
实例1
将29.3g的苯胺加入100ml自来水和130ml1+1盐酸，搅拌均匀，形成盐酸苯胺溶液，在0～5℃将27%的亚硝酸钠溶液滴加到上述溶液中，用新制备的碘化钾淀粉试纸测定反应终点，得到重氮组份溶液。
偶合组份溶液是将35ml，40%的烧碱和15g红油溶于250ml自来水中，加热至90℃，加入84g色酚AS，搅拌使之完全溶解，然后稀释，得到体积为1400ml的偶合组份溶液。
将超细滑石粉60g（1～5μ），加水制成料浆，注入到偶合组份溶液中，搅拌均匀。温度保持在45±5℃，滴入重氮组份，速度为20ml/min，进行偶合反应，保持温度基本不变，反应毕再经过滤洗涤、干燥、粉碎。所得产品色光与标准品相近似，着色力为纯大红粉的80%，吸油值45%，水溶物小于1.0%，耐光性不低于6级。
实例2
制备方法同实例1，成核材料为超细膨润土60g，偶合温度控制在30±2℃，重氮液加入速度为40ml，时间15分钟。产品性能为：色光与标准品相似，着色力为纯大红粉的75%，吸油值47%，水溶物小于1.0%，耐光性不低于6级。
实例3
制备方法同实例1，成核材料为超细高岭土60g，偶合温度控制在50±2℃，重氮液加入速度为30ml/min，时间20分钟。产品性能为：色光与标准品相近似，着色力为纯大红粉的80%，吸油值42%，水溶物小于1.0%，耐光性不低于6级。
实例4
制备方法同实例1，成核材料为超细二氧化硅60g，偶合反应温度控制在55±2℃，重氮液加入速度为60ml/min，时间为10分钟。产品性能为：色光与标准品相似，着色力为纯大红粉的80%，吸油值50%，水溶物小于1.0%，耐光性不低于6级。
Claims (4)
1、一种制造红色有机--无机包核颜料的方法，是将苯胺加入自来水和1+1盐酸中，搅拌均匀，加入碎冰冷却至0℃左右，搅拌下滴加27%亚硝酸钠溶液，在5℃下进行重氟反应，得到重氟组份溶液，将40%的烧碱和红油溶于自来水中，加热至90℃，加入色酚AS，搅拌均匀，然后加水稀释得到浓度为5～7%的偶合组份溶液，将超细无机体质颜料以0.5∶1的比例加入到偶合组份溶液中，然后在搅拌下将重氮组份溶液慢慢加入到含有超细无机体质颜料的偶合溶液中，进行偶合反应，控制反应温度30～60℃，时间10～30分钟，PH值8～12，然后过滤、洗涤、干燥、粉碎。
2、一种如权利要求1所述的方法，其特征是所说的无机体质颜料的粒度分布在1～5μ，加入量为无机体质颜料∶偶合组份溶液＝0.5∶1.0。
3、一种如权利要求1所述的方法，其特征是所说的无机体质颜料可以是超细滑石粉、超细二氧化硅、超细高岭土、超细膨润土。
4、一种如权利要求所述的方法，其特征是重氮组份溶液与偶合组份溶液的体积比为1∶2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111775 CN1073463A (zh) | 1991-12-18 | 1991-12-18 | 红色有机-无机包核颜料 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91111775 CN1073463A (zh) | 1991-12-18 | 1991-12-18 | 红色有机-无机包核颜料 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1073463A true CN1073463A (zh) | 1993-06-23 |
Family
ID=4910839
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91111775 Pending CN1073463A (zh) | 1991-12-18 | 1991-12-18 | 红色有机-无机包核颜料 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1073463A (zh) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277010A (zh) * | 2011-05-05 | 2011-12-14 | 天津城市建设学院 | 无机核-壳材料双修饰改性大红粉的制备方法 |
| EP3561003A1 (en) | 2018-04-23 | 2019-10-30 | Clariant Plastics & Coatings Ltd | A hybrid pigment, method for preparation thereof and uses thereof |
-
1991
- 1991-12-18 CN CN 91111775 patent/CN1073463A/zh active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277010A (zh) * | 2011-05-05 | 2011-12-14 | 天津城市建设学院 | 无机核-壳材料双修饰改性大红粉的制备方法 |
| EP3561003A1 (en) | 2018-04-23 | 2019-10-30 | Clariant Plastics & Coatings Ltd | A hybrid pigment, method for preparation thereof and uses thereof |
| WO2019206697A1 (en) | 2018-04-23 | 2019-10-31 | Clariant Plastics & Coatings Ltd | A hybrid pigment, method for preparation thereof and uses thereof |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
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