CN113072824A - Modification method of special heavy calcium carbonate for bulk molding compound - Google Patents
Modification method of special heavy calcium carbonate for bulk molding compound Download PDFInfo
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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
- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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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- 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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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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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- 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
- C09C3/12—Treatment with organosilicon compounds
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- 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
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- 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
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- 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
- C01P2006/90—Other properties not specified above
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
Abstract
The invention provides a modification method of special heavy calcium carbonate for bulk molding compounds, which comprises the following steps: s1, melting oxidized polyethylene wax and mixing with pentaerythritol stearate to obtain a stock solution I; mixing a silane coupling agent and hydroxyethyl acrylate to obtain a stock solution II; s2, mixing the stock solution II with heavy calcium carbonate, and uniformly stirring to obtain an initial mixture; s3, adding the initial mixture into the stock solution I, and uniformly stirring to obtain a mixture; and S4, feeding the mixture into a mill for grinding to obtain the modified special heavy calcium carbonate for the bulk molding compound. According to the method, the silane coupling agent, the hydroxyethyl acrylate, the pentaerythritol stearate and the oxidized polyethylene wax are mixed and then added into a mill for grinding modification, so that the oil absorption value of the heavy calcium carbonate can be reduced, the filling ratio in the bulk molding compound is improved, the viscosity coefficient and the extrusion current are reduced, the screw abrasion is reduced, the product percent of pass is improved, and the production efficiency of powder is improved.
Description
Technical Field
The invention relates to the field of heavy calcium carbonate production, in particular to a modification method of special heavy calcium carbonate for bulk molding compounds.
Background
BMC (bulk molding compound) or DMC (multi-wall molding compound) is called bulk molding compound (formerly BT-3), and like sheet molding compounds, is a chopped fiber reinforced thermoset molding compound. Today in the united states, japan and china, BMC and DMC are usually the same material, BMC being chemically thickened DMC according to the definition of SPI in the united states. The composite material can be processed by die pressing, transfer molding, injection molding and the like, and the prepared product has the advantages of good mechanical property, high dimensional stability, good surface smoothness, excellent water resistance, oil resistance and corrosion resistance, heat resistance and excellent electrical property, and particularly the arc resistance can reach about 190 s.
In the production process of Bulk Molding Compounds (BMC), heavy calcium carbonate is usually adopted as a filler, but the heavy calcium carbonate has a high oil absorption value, a large system viscosity, a low filling proportion and high cost, the manufactured product has low impact resistance and a large deformation coefficient, and the glass fiber is easily peeled from other materials in the injection molding and extrusion process to cause uneven filling, so that the product size and the stability of various properties are influenced.
Although the prior art has more reports on the modification of the heavy calcium carbonate, most of the heavy calcium carbonate only aims at the oil absorption value, the viscosity coefficient and the filling proportion in the bulk molding compound are not considered, and even if the oil absorption value is very low, the production of the bulk molding compound is difficult to adapt, so that the product percent of pass is too low.
Disclosure of Invention
The invention aims to solve the problems and provide a method for modifying heavy calcium carbonate special for bulk molding compounds, which can reduce the oil absorption value of the heavy calcium carbonate and improve the filling ratio in the bulk molding compounds, thereby improving the product yield.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a modification method of heavy calcium carbonate special for bulk molding compound comprises the following steps:
s1, melting oxidized polyethylene wax and mixing with pentaerythritol stearate to obtain a stock solution I; and mixing the silane coupling agent and hydroxyethyl acrylate to obtain stock solution II.
S2, mixing the stock solution II with the heavy calcium carbonate, and uniformly stirring to obtain an initial mixture.
And S3, adding the initial mixture into the stock solution I, and uniformly stirring to obtain a mixture.
And S4, feeding the mixture into a mill for grinding to obtain the modified special heavy calcium carbonate for the bulk molding compound.
Preferably, in step S1, the oxidized polyethylene wax is melted at 65-75 ℃.
Preferably, in step S1, the silane coupling agent is a silane coupling agent KH 550.
Preferably, in step S1, the pentaerythritol stearate is added in an amount of 0.05 to 0.2% by mass of the ground calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.05-0.2%.
Preferably, in step S1, the silane coupling agent is added in an amount of 0.1 to 0.3% by mass of ground calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.1-0.3%.
Preferably, in step S4, the slurry mixture is fed into a mill for grinding, the grinding temperature is controlled at 35-45 ℃, and the slurry mixture is ground to a fineness of 200-300 meshes.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
1. according to the modification method of the special heavy calcium carbonate for the bulk molding compound, the silane coupling agent, the hydroxyethyl acrylate, the pentaerythritol stearate and the oxidized polyethylene wax are mixed and then added into a mill for grinding modification, so that the oil absorption value of the heavy calcium carbonate can be reduced, the filling ratio in the bulk molding compound is improved, the viscosity coefficient and the extrusion current are reduced, the screw abrasion is reduced, the product percent of pass is improved, the production efficiency of powder is improved, and the production cost is reduced.
2. The modification method of the special heavy calcium carbonate for bulk molding compounds adopts the modifier, and the silane coupling agent mainly has the effects of increasing the compatibility of calcium carbonate and unsaturated resin, shortening the stirring time to improve the production efficiency, reducing the oil absorption value of calcium carbonate powder and increasing the filling proportion after reacting with the calcium carbonate to play a coupling role, and simultaneously, the silane coupling agent can also have a very strong coupling effect with glass fibers to reduce the separation of the glass fibers.
The pentaerythritol stearate has the effects of increasing the thixotropy of a system, reducing the viscosity and extrusion pressure of the system, enabling the coated glass fibers with better melting bodies to enter a die together when extrusion filling is carried out, and ensuring more compact filling and higher glossiness.
The hydroxyethyl acrylate plays a role in coupling, and due to the active hydroxyl functional groups, the hydroxyethyl acrylate can perform anchoring reaction with calcium carbonate at the moment of crushing and molecular bond breaking, and the active functional groups and the silane coupling agent have synergistic effect, so that the requirement of auxiliary agent modification on temperature is reduced.
Oxidized polyethylene wax contains a certain amount of carboxyl and hydroxyl in molecules, reacts with calcium carbonate to increase compatibility, shortens system plasticizing time, reduces torque, increases melt fluidity, improves demolding and increases yield; the glossiness of the finished product is improved, and the appearance is improved.
3. The method for modifying the heavy calcium carbonate special for the bulk molding compound has the advantages of simple process and higher efficiency, only needs to be carried out at the temperature of 35-45 ℃, reduces the production cost, and is worthy of industrial popularization.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A modification method of heavy calcium carbonate special for bulk molding compound comprises the following steps:
s1, melting oxidized polyethylene wax at 70 ℃ and mixing the oxidized polyethylene wax with pentaerythritol stearate to obtain a stock solution I; and mixing the silane coupling agent and hydroxyethyl acrylate to obtain stock solution II.
S2, mixing the stock solution II with the heavy calcium carbonate, and uniformly stirring to obtain an initial mixture.
And S3, adding the initial mixture into the stock solution I, and uniformly stirring to obtain a mixture.
S4, feeding the mixture into a mill for grinding, controlling the grinding temperature at 35 ℃, and grinding to the fineness of 200 meshes to obtain the modified special heavy calcium carbonate for the bulk molding compound.
The addition amount of the pentaerythritol stearate is 0.2 percent based on the mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.05 percent.
The adding amount of the silane coupling agent is 0.3 percent based on the mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.1 percent.
Example 2
A modification method of heavy calcium carbonate special for bulk molding compound comprises the following steps:
s1, melting oxidized polyethylene wax at 70 ℃ and mixing the oxidized polyethylene wax with pentaerythritol stearate to obtain a stock solution I; and mixing the silane coupling agent and hydroxyethyl acrylate to obtain stock solution II.
S2, mixing the stock solution II with the heavy calcium carbonate, and uniformly stirring to obtain an initial mixture.
And S3, adding the initial mixture into the stock solution I, and uniformly stirring to obtain a mixture.
S4, feeding the mixture into a mill for grinding, controlling the grinding temperature at 40 ℃, and grinding to the fineness of 250 meshes to obtain the modified special heavy calcium carbonate for the bulk molding compound.
The addition amount of the pentaerythritol stearate is 0.1 percent based on the mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.1 percent.
The adding amount of the silane coupling agent is 0.2 percent based on the mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.2 percent. The silane coupling agent is a silane coupling agent KH550
Example 3
A modification method of heavy calcium carbonate special for bulk molding compound comprises the following steps:
s1, melting oxidized polyethylene wax at 70 ℃ and mixing the oxidized polyethylene wax with pentaerythritol stearate to obtain a stock solution I; and mixing the silane coupling agent and hydroxyethyl acrylate to obtain stock solution II.
S2, mixing the stock solution II with the heavy calcium carbonate, and uniformly stirring to obtain an initial mixture.
And S3, adding the initial mixture into the stock solution I, and uniformly stirring to obtain a mixture.
S4, feeding the mixture into a mill for grinding, controlling the grinding temperature at 45 ℃, and grinding to the fineness of 250 meshes to obtain the modified special heavy calcium carbonate for the bulk molding compound.
The addition amount of the pentaerythritol stearate is 0.05 percent based on the mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.05 percent.
The adding amount of the silane coupling agent is 0.1 percent based on the mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.1 percent.
And (3) experimental verification:
the verification method comprises the following steps: different heavy calcium carbonates are adopted to prepare bulk molding compounds, and the filling amount, pasting time, viscosity coefficient, glossiness, dimensional tolerance, bending strength, powder production efficiency, extrusion production efficiency, screw extrusion current and product percent of pass are recorded and calculated to verify the modification effect of the heavy calcium carbonates.
Preparing a bulk molding compound, comprising the following steps:
s1, adding the composite resin, the curing agent, the release agent and the auxiliary agent into a stirrer, uniformly stirring at a high speed, then adding the ground limestone, mixing and stirring, defoaming in vacuum, and discharging to obtain the resin premix.
S2, adding the premix into a biaxial kneading machine, adding the dried reinforced fibers, kneading, pouring out a dough, extruding by an extruder, and drying to obtain a bulk molding compound.
Experimental groups were as follows:
experimental example 1 unmodified ground calcium carbonate was used.
Experimental example 2 the ground calcium carbonate prepared in example 2 was used.
Compared with the method of experimental example 2, the method of calcium carbonate modification adopted in experimental example 3 only adopts silane coupling agent, hydroxyethyl acrylate and oxidized polyethylene wax, and the addition amount and other steps are the same as those of experimental example 2.
Experimental example 4 compared with the method of experimental example 2, the method of modifying calcium carbonate used only includes silane coupling agent, pentaerythritol stearate and polyethylene oxide wax, and the addition amount and other steps are the same as those of experimental example 2.
Experimental example 5 compared with the method of modifying calcium carbonate in Experimental example 2, the method of modifying calcium carbonate only adopts silane coupling agent, pentaerythritol stearate and hydroxyethyl acrylate, and the addition amount and other steps are the same as those of the method of experimental example 2.
The heavy calcium carbonate is 250 meshes.
Experimental data:
and recording and calculating the filling amount, the pasting time, the viscosity coefficient, the glossiness, the dimensional tolerance, the bending strength, the powder production efficiency, the extrusion production efficiency, the screw extrusion current and the product percent of pass.
Through multiple experimental comparisons: experiment 1, adopting unmodified ground calcium carbonate, wherein the filling amount reaches 60 percent to the maximum, and experiment 2, the filling amount of the ground calcium carbonate reaches 78 percent to the maximum; experiments 3-5, the maximum filling amount respectively reaches 73%, 72% and 74%;
the data are summarized in tables 1 and 2 below:
table 1 injection molding extrusion data
TABLE 2 powder and BMC data
Discussion of the results:
as can be seen from tables 1 and 2, the oil absorption value of the unmodified heavy calcium powder is 20, the filling ratio is only 60%, the viscosity coefficient is as high as 500000, the extrusion current is 38A, the abrasion of the screw is serious, and the screw fittings are replaced basically for 8 months. The product percent of pass is only 85.6 percent.
With the heavy calcium powder prepared in experimental example 2, the oil absorption value was 15, the filling ratio was increased to 78%, the viscosity coefficient was reduced to 384920, the extrusion current was reduced to 30A, the screw wear was reduced, and the screw part replacement time was extended to 18 months. The product percent of pass is improved to 99.8 percent. Meanwhile, the production efficiency of the powder is greatly improved, and the production cost is greatly reduced.
Experimental examples 3-4 show that the calcium carbonate is used for reacting to play a synergistic role in the aspects of coupling, increasing compatibility, increasing thixotropy of a system and the like, so that the viscosity and extrusion pressure of the system are reduced, the plasticizing time is shortened, the torque is reduced, the fluidity of a melt is increased, the demolding is improved, and the yield is increased; the glossiness of the finished product is improved, and the appearance is improved. The effect is obviously reduced by lacking any component.
The above description is directed to the details of the preferred and possible embodiments of the present invention, but the embodiments are not intended to limit the scope of the claims of the present invention. All changes and modifications that come within the spirit of the invention are desired to be protected.
Claims (6)
1. A modification method of special heavy calcium carbonate for bulk molding compounds is characterized by comprising the following steps:
s1, melting oxidized polyethylene wax and mixing with pentaerythritol stearate to obtain a stock solution I; mixing a silane coupling agent and hydroxyethyl acrylate to obtain a stock solution II;
s2, mixing the stock solution II with heavy calcium carbonate, and uniformly stirring to obtain an initial mixture;
s3, adding the initial mixture into the stock solution I, and uniformly stirring to obtain a mixture;
and S4, feeding the mixture into a mill for grinding to obtain the modified special heavy calcium carbonate for the bulk molding compound.
2. The method for modifying heavy calcium carbonate specially used for bulk molding compounds as claimed in claim 1, wherein in step S1, the oxidized polyethylene wax is melted at 65-75 ℃.
3. The method for modifying bulk molding compound-specific ground calcium carbonate according to claim 1, wherein in step S1, the silane coupling agent is KH 550.
4. The method for modifying heavy calcium carbonate specially used for bulk molding compounds as claimed in claim 1, wherein in step S1, the amount of pentaerythritol stearate added is 0.05-0.2% by mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.05-0.2%.
5. The method for modifying heavy calcium carbonate specially used for bulk molding compounds as claimed in claim 1, wherein in step S1, the amount of the silane coupling agent added is 0.1-0.3% by mass of the heavy calcium carbonate; the addition amount of the oxidized polyethylene wax is 0.1-0.3%.
6. The method for modifying heavy calcium carbonate specially used for bulk molding compounds as claimed in claim 1, wherein in step S4, the slurry mixture is sent to a mill for grinding, the grinding temperature is controlled at 35-45 ℃, and the ground mixture is ground to a fineness of 200-300 meshes.
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|---|---|---|---|---|
| SU1647019A1 (en) * | 1989-01-10 | 1991-05-07 | Предприятие П/Я А-3732 | Process for modifying carbonate filler |
| CN104087027A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | High-temperature-resistant modified calcium carbonate and preparation method thereof |
| CN106751864A (en) * | 2016-12-26 | 2017-05-31 | 广西贺州市科隆粉体有限公司 | The modified powdered whiting of a kind of surface modifying method of special powdered whiting of silicone adhesive and surface |
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| CN109337243A (en) * | 2018-09-28 | 2019-02-15 | 贺州钟山县双文碳酸钙新材料有限公司 | Utilize the PVC calcium-plastic board material and preparation method thereof of modified calcium carbonate enhancing |
-
2021
- 2021-03-29 CN CN202110335349.0A patent/CN113072824B/en active Active
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| SU1647019A1 (en) * | 1989-01-10 | 1991-05-07 | Предприятие П/Я А-3732 | Process for modifying carbonate filler |
| CN104087027A (en) * | 2014-06-06 | 2014-10-08 | 凤台县精华助剂有限公司 | High-temperature-resistant modified calcium carbonate and preparation method thereof |
| CN106751864A (en) * | 2016-12-26 | 2017-05-31 | 广西贺州市科隆粉体有限公司 | The modified powdered whiting of a kind of surface modifying method of special powdered whiting of silicone adhesive and surface |
| CN108892995A (en) * | 2018-05-24 | 2018-11-27 | 贺州钟山县双文碳酸钙新材料有限公司 | A kind of method of modifying of car paint color inhibition calcium carbonate |
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| Title |
|---|
| 王善勤主编: "《塑料配方设计问答》", 31 January 2003, 北京：中国轻工业出版社 * |
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