CN116023802A - Modified heavy calcium carbonate with low oil absorption value - Google Patents
Modified heavy calcium carbonate with low oil absorption value Download PDFInfo
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- CN116023802A CN116023802A CN202211685180.2A CN202211685180A CN116023802A CN 116023802 A CN116023802 A CN 116023802A CN 202211685180 A CN202211685180 A CN 202211685180A CN 116023802 A CN116023802 A CN 116023802A
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- CN
- China
- Prior art keywords
- calcium carbonate
- heavy calcium
- oil absorption
- absorption value
- modified heavy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 123
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 61
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 30
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 19
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 19
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000008117 stearic acid Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- KQHKITXZJDOIOD-UHFFFAOYSA-M sodium;3-sulfobenzoate Chemical compound [Na+].OS(=O)(=O)C1=CC=CC(C([O-])=O)=C1 KQHKITXZJDOIOD-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- DLYROBIGGZFBOQ-UHFFFAOYSA-N carboxy benzenesulfonate Chemical compound OC(=O)OS(=O)(=O)C1=CC=CC=C1 DLYROBIGGZFBOQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- QMWGSOMVXSRXQX-UHFFFAOYSA-N 3-sulfobenzoic acid Chemical compound OC(=O)C1=CC=CC(S(O)(=O)=O)=C1 QMWGSOMVXSRXQX-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 30
- 230000004048 modification Effects 0.000 abstract description 12
- 238000012986 modification Methods 0.000 abstract description 12
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000004094 surface-active agent Substances 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 4
- 229940077386 sodium benzenesulfonate Drugs 0.000 abstract description 4
- 239000000843 powder Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 239000003607 modifier Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- -1 papermaking Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000004579 marble Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229940034610 toothpaste Drugs 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a modified heavy calcium carbonate with a low oil absorption value, which relates to the technical field of heavy calcium carbonate modification, and is prepared by heating heavy calcium carbonate, sequentially adding sodium 3-carboxybenzenesulfonate and stearic acid into the heavy calcium carbonate in the heating process, and stirring for reaction. The invention adopts a dry process, adopts the surfactant of 3-carboxyl sodium benzenesulfonate and stearic acid to modify the heavy calcium carbonate, and the oil absorption value of the obtained heavy calcium carbonate can reach 20.6mg/100g, and the preparation method is simple and the cost is low.
Description
Technical Field
The invention relates to the technical field of heavy calcium carbonate modification, in particular to modified heavy calcium carbonate with a low oil absorption value.
Background
The heavy calcium carbonate is a calcium carbonate powder material produced by adopting the mechanical crushing method and taking ores such as calcite, chalk, marble and the like as raw materials, has the characteristics of wide raw material source, high whiteness, low oil absorption value, good applicability, low price and the like, is inorganic nonmetallic mineral powder with the widest application and the largest dosage at present, is generally used as a filler, and is widely used in daily chemical industries such as artificial floor tiles, rubber, plastics, papermaking, paint, printing ink, cables, building products, foods, medicines, textiles, feeds, toothpaste and the like, and the filler plays a role of increasing the volume of products, reducing the production cost, and improving the physical properties such as dimensional stability, mechanical properties and the like of the materials.
The oil absorption value affects the dispersibility of heavy calcium carbonate in filler materials or articles and the processability (ease of mixing) of the filler resin system, and affects the dispersion stability or sedimentation properties of paints and inks. The oil absorption value of the existing heavy calcium carbonate is about 48ml/100g, and the heavy calcium carbonate needs to be modified to further reduce the oil absorption value. In the prior art, different kinds of modifiers are often used for modifying the calcium carbonate powder, such as titanate coupling agents, stearic acid, sodium dodecyl benzene sulfonate, stearic acid, titanate coupling agents, silane coupling agents, polymethyl methacrylate and other composite modifiers. However, the modification effect is poor, the process condition is not well controlled, and the powder yellowing and the like are problems.
At present, the production of heavy calcium carbonate in China mainly comprises a dry process and a wet process. The modification of calcium carbonate is also mainly involved in both processes. The wet modification is mainly to put the ground powder into a modifier aqueous solution, and obtain the modified water-based modified polyurethane through mixing, stirring, dehydrating and drying. The modification method has high cost and insignificant effect. The dry modification process is to put the ground heavy calcium into modification equipment such as a ball mill, a high-speed kneader, an air classifier and the like, and add a modifier for modification. However, dry modification processes are often used for modification of light calcium carbonate, with the aim of increasing the activation rate of the calcium carbonate powder.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the modified heavy calcium carbonate with low oil absorption value, which is prepared by modifying the heavy calcium carbonate by selecting the surfactant sodium 3-carboxybenzenesulfonate and stearic acid, and the two are synergistic to obtain the heavy calcium carbonate with low oil absorption value.
The modified heavy calcium carbonate with low oil absorption value provided by the invention is heated, and in the heating process, 3-sodium carboxybenzenesulfonate and stearic acid are sequentially added into the heavy calcium carbonate, and the mixture is stirred and reacted to obtain the modified heavy calcium carbonate with low oil absorption value.
Preferably, the addition amount of the 3-carboxybenzene sulfonic acid is 0.1 to 0.3 weight percent of the weight of the heavy calcium carbonate respectively.
Preferably, the stearic acid is added in an amount of 0.2 to 0.6wt% of the weight of the heavy calcium carbonate, respectively.
Preferably, the heavy calcium carbonate is heated to 100-115 ℃, and 3-carboxyl sodium benzenesulfonate is added in the heating process, and stearic acid is added after the heating to 100-115 ℃, and stirring reaction is carried out for 3-5 min.
Preferably, the heating is carried out to 100-115 ℃ at a heating rate of 13.5-15.5 ℃/min.
The beneficial effects are that: according to the invention, a dry process is adopted, and surfactants of 3-sodium carboxybenzenesulfonate and stearic acid are selected to modify the heavy calcium carbonate, and the two surfactants are synergistic, so that the 3-sodium carboxybenzenesulfonate is adsorbed on the surface of the calcium carbonate powder to play a role in dispersing the calcium carbonate powder, thereby facilitating the adsorption between the stearic acid and the calcium carbonate powder, and the oil absorption value of the obtained heavy calcium carbonate can reach 20.6mg/100g, and the preparation method is simple and low in cost.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
Example 1
The preparation method of the modified heavy calcium carbonate comprises the following steps:
(1) 1000kg of heavy calcium carbonate powder is added into stirring equipment and heated at a temperature of 15 ℃/min;
(2) 2.0kg of sodium 3-carboxybenzenesulfonate is added when the stirring equipment is heated to 70 ℃;
(3) When the stirring equipment is heated to 110 ℃, adding 4.0kg of stearic acid, and stirring for 4min;
(4) And (5) turning off the stirring equipment, waiting for the material to cool, discharging, and detecting the oil absorption value of the material to reach 20.6mL/100g.
Example 2
The preparation method of the modified heavy calcium carbonate comprises the following steps:
(1) 1000kg of heavy calcium carbonate powder is added into stirring equipment and heated at a temperature of 15 ℃/min;
(2) 2.2kg of sodium 3-carboxybenzenesulfonate are added when the stirring equipment is heated to 80 ℃;
(3) When the stirring equipment is heated to 110 ℃, adding 4.8kg of stearic acid, and stirring for 5min;
(4) And (5) turning off the stirring equipment, waiting for the material to cool, discharging, and detecting the oil absorption value of the material to reach 20.8mL/100g.
Example 3
The preparation method of the modified heavy calcium carbonate comprises the following steps:
(1) 1000kg of heavy calcium carbonate powder is added into stirring equipment and heated at a temperature of 13.5 ℃/min;
(2) When the stirring equipment is heated to 50 ℃, 1.0kg of 3-carboxyl sodium benzenesulfonate is added;
(3) When the stirring equipment is heated to 100 ℃, adding 2.0kg of stearic acid, and stirring for 4min;
(4) And (5) turning off the stirring equipment, waiting for the material to cool, discharging, and detecting the oil absorption value of the material to reach 20.4mL/100g.
Example 4
The preparation method of the modified heavy calcium carbonate comprises the following steps:
(1) 1000kg of heavy calcium carbonate powder is added into stirring equipment and heated at a temperature of 15.5 ℃/min;
(2) 3.0kg of sodium 3-carboxybenzenesulfonate is added when the stirring equipment is heated to 90 ℃;
(3) When the stirring equipment is heated to 115 ℃, adding 6.0kg of stearic acid, and stirring for 5min;
(4) And (5) turning off the stirring equipment, waiting for the material to cool, discharging, and detecting the oil absorption value of the material to reach 20.7mL/100g.
Comparative example 1
The preparation method of the modified heavy calcium carbonate comprises the following steps:
(1) 1000kg of heavy calcium carbonate powder is added into stirring equipment and heated at a temperature of 15 ℃/min;
(2) When the stirring equipment is heated to 110 ℃, adding 4.0kg of stearic acid, and stirring for 4min;
(3) The stirring equipment is closed, the materials are cooled, discharged and the oil absorption value is detected to be 23.0mL/100g.
Comparative example 2
The preparation method of the modified heavy calcium carbonate comprises the following steps:
(1) 1000kg of heavy calcium carbonate powder is added into stirring equipment and heated at a temperature of 15 ℃/min;
(2) When the stirring equipment is heated to 70 ℃, 2.0kg of 3-carboxyl sodium benzenesulfonate is added, and then the mixture is heated to 110 ℃ and stirred for 4min;
(3) The stirring equipment is closed, the materials are cooled, discharged and the oil absorption value is detected to be 30.0mL/100g.
The oil absorption value of the modified heavy calcium carbonate prepared in the embodiment 1-4 of the invention is 20.4-20.8mL/100 g. By detecting the oil absorption values of the modified calcium carbonate prepared in example 1 and comparative example 1, it can be seen that the modification effect of calcium carbonate by using single stearic acid is poor and the oil absorption value is high; in contrast, in comparative example 2, a single sodium 3-carboxybenzenesulfonate salt was used, which also had a higher oil absorption value; the 2 surfactants are compounded to realize synergistic effect, and the oil absorption value of the modified heavy calcium carbonate is lower.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. The modified heavy calcium carbonate with low oil absorption value is characterized in that the modified heavy calcium carbonate is heated, and in the heating process, 3-sodium carboxybenzenesulfonate and stearic acid are sequentially added into the heavy calcium carbonate, and the mixture is stirred and reacted to obtain the modified heavy calcium carbonate.
2. The modified heavy calcium carbonate of low oil absorption value according to claim 1, wherein the 3-carboxybenzenesulfonic acid is added in an amount of 0.1 to 0.3wt% of the weight of the heavy calcium carbonate, respectively.
3. The modified heavy calcium carbonate of low oil absorption value according to claim 1 or 2, wherein the stearic acid is added in an amount of 0.2 to 0.6wt% of the weight of the heavy calcium carbonate, respectively.
4. A modified heavy calcium carbonate with low oil absorption value according to any one of claims 1-3, wherein the heavy calcium carbonate is heated to 100-115 ℃, and sodium 3-carboxybenzenesulfonate is added during the heating process, and stearic acid is added after the heating to 100-115 ℃, and the reaction is stirred for 3-5 min.
5. The modified heavy calcium carbonate of low oil absorption according to claim 4, wherein the heavy calcium carbonate is heated to 100 to 115 ℃ at a heating rate of 13.5 to 15.5 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211685180.2A CN116023802A (en) | 2022-12-27 | 2022-12-27 | Modified heavy calcium carbonate with low oil absorption value |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211685180.2A CN116023802A (en) | 2022-12-27 | 2022-12-27 | Modified heavy calcium carbonate with low oil absorption value |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116023802A true CN116023802A (en) | 2023-04-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211685180.2A Pending CN116023802A (en) | 2022-12-27 | 2022-12-27 | Modified heavy calcium carbonate with low oil absorption value |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116023802A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116925573A (en) * | 2023-07-20 | 2023-10-24 | 浙江钦堂钙业有限公司 | Activated modified heavy calcium carbonate and preparation method thereof |
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2022
- 2022-12-27 CN CN202211685180.2A patent/CN116023802A/en active Pending
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