CN111574852A - Preparation method of active heavy calcium carbonate - Google Patents
Preparation method of active heavy calcium carbonate Download PDFInfo
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- CN111574852A CN111574852A CN202010504421.3A CN202010504421A CN111574852A CN 111574852 A CN111574852 A CN 111574852A CN 202010504421 A CN202010504421 A CN 202010504421A CN 111574852 A CN111574852 A CN 111574852A
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- 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
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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- 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
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- 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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- 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
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/90—Other properties not specified above
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Abstract
The invention discloses a preparation method of active heavy calcium carbonate, which comprises the following steps: carrying out two-stage turbine airflow classification on the heavy calcium carbonate, wherein the granularity range of the fine powder product obtained after classification is obviously narrowed, and the granularity is reduced; collecting powder by adopting a chamber-divided powder collecting technology; adding the collected powder into the reaction kettle, controlling the temperature at 110 ℃ and stirring; then adding the assistant 1, controlling the temperature at 120-130 ℃, and stirring. Adding the auxiliary agent 2 into the reaction kettle, controlling the temperature at 135-140 ℃, and stirring to obtain the active heavy calcium carbonate. According to the invention, the double auxiliaries are adopted for composite treatment, so that different types of substances can be organically combined together in the production and processing of the adhesive, and the product quality and stability are improved.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a preparation method of active heavy calcium carbonate.
Background
The adhesive product is widely applied to the industries of buildings, electronic instruments and meters and parts. In recent years, with the rapid development of the door and window market of buildings, the market demand of adhesives is continuously increased, the adhesive industry is stepped into a developed express way, the using amount is greatly increased, the product variety is more and more perfect, the product quality demand of people on adhesives is higher and higher, and common domestic adhesives cannot meet the demand, so that the adhesives imported from Japan can be rapidly worn in the Chinese market, and numerous consumers are very favored. The mainstream products of the adhesive are polysulfide adhesive and silicone adhesive, but the polysulfide adhesive has an environmental protection problem, so the usage rate is lower and lower, and the silicone adhesive has no environmental protection problem and the cost is greatly reduced, so the main product of the adhesive is trending.
The calcium carbonate has the characteristics of narrow particle size distribution, high whiteness and good dispersion effect, is widely used as a filling material of an adhesive, has the advantages of easily available raw materials, low price, good stability, simple color, no toxicity and the like, is widely used in the fields of plastics, rubber, papermaking, printing ink, building materials, electric wires, cables and the like, and becomes a filling material with the largest using amount. However, calcium carbonate belongs to inorganic powder, the particle surface is hydrophilic and oleophobic and is strong in polarity, the calcium carbonate is difficult to disperse uniformly in an organic medium, the binding force between the calcium carbonate and a base material is low, and interface defects are easily caused when the calcium carbonate is impacted by external force, so that the performance of the material is reduced; the nano calcium carbonate powder has high surface energy and stronger adsorption, and the particles are mutually agglomerated and cannot be well dispersed in a polymer matrix, so that the practical use effect of the nano calcium carbonate powder is influenced. The current heavy calcium carbonate modification technology has little difference at home and abroad, but has a difference in modification quality control, the current surface preparation method of the calcium carbonate mainly adopts chemical coating assisted with mechanochemistry, and the used surface modifiers comprise stearic acid (salt), titanate coupling agent, aluminate coupling agent and the like.
The existing filler product special for the adhesive has the following problems: the particle size distribution is wide, and the elasticity performance of the adhesive product is influenced; the whiteness is low, so that the glossiness of the product is influenced; the dispersibility in the adhesive is poor.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention adopts a novel production process of the special material for the adhesive, and the product prepared by the method has good dispersion effect in the adhesive, can replace resin to a great extent, and reduces the cost.
The technical scheme is as follows: the preparation method of the active heavy calcium carbonate provided by the invention comprises the following steps:
step 1: carrying out two-stage turbine airflow classification on the heavy calcium carbonate, wherein the granularity range of the fine powder product obtained after classification is obviously narrowed, and the granularity is reduced;
step 2: the powder collection is carried out by adopting a chamber-divided powder collection technology, the dust removed from the powder collection chamber has enough time to fall into the ash hopper, and the probability of flying again is very small; the ash removal frequency is reduced, and the ash removal efficiency is high; the compressed air quantity required by the ash removal is less, so that the electric energy is saved;
and step 3: adding the powder collected in the step 1 into a reaction kettle, controlling the temperature at 100 ℃ and 110 ℃, and stirring;
and 4, step 4: then adding the assistant 1, controlling the temperature at 120-130 ℃, and stirring.
And 5: adding the auxiliary agent 2 into the reaction kettle, controlling the temperature at 135 ℃ and 140 ℃, and stirring to obtain the active heavy calcium carbonate;
wherein the auxiliary agent 1 is stearate, and the auxiliary agent 2 is aluminate;
the weight ratio of the heavy calcium carbonate to the auxiliary agent 1 to the auxiliary agent 2 is (100: 0.2-1): 0.2-1.
Specifically, the two-stage turbine airflow classification adopts a narrow-level two-stage turbine airflow classifier, and is realized by connecting two turbine airflow classifiers in series.
Specifically, the chamber-divided powder collecting technology is provided with a plurality of powder collecting chambers, and the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by a controller to realize the switching of the working states of the powder collecting chambers, so that off-line ash removal can be realized.
Preferably, the weight part ratio of the heavy calcium carbonate to the auxiliary agent 1 to the auxiliary agent 2 is 100: 0.5: 0.5.
preferably, the stirring speed of the step 3 and the step 4 is greater than the stirring speed of the step 3.
Preferably, the stirring time of the step 3, the step 4 and the step 5 is 2-5 min.
Preferably, the temperature of the step 3 is controlled at 105 ℃, and the stirring time is 3 min; the temperature of the step 4 is controlled at 125 ℃, and the stirring time is 3 min; and in the step 5, the temperature is controlled at 135 ℃, and the stirring time is 3 min.
Preferably, the particle diameter of the heavy calcium carbonate is less than or equal to 6 μm, wherein the content of particles with the particle diameter of less than 2 μm accounts for more than 32 percent of the total content.
Has the advantages that:
(1) stearic acid and a coupling agent are adopted for composite treatment, so that different types of substances can be organically combined together in the production and processing of the adhesive, and the quality and stability of the product are improved;
(2) a narrow-level two-stage turbine airflow classifier grading system is adopted to effectively carry out two-stage grading on the materials, and the granularity range of the fine powder product obtained after grading is obviously narrowed, the granularity is reduced, and the requirement of the modern on the narrow level of the powder is met;
(3) the self-chambering powder collecting device is adopted, a plurality of powder collecting chambers are arranged through design, and the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working states of the powder collecting chambers, so that offline ash removal can be realized, the powder collecting efficiency is improved, and the energy consumption is saved.
(4) The product has the characteristics of narrow particle size distribution, high whiteness, good dispersion effect and the like, can replace resin, and reduces the cost. After the product is modified, the oil absorption value is low, and the dispersion effect in the adhesive is good. Compared with common fillers, the adhesive has improved adhesive bonding force.
(5) The special material for modified calcium carbonate prepared by the method is mainly used as a filler of an adhesive, so that the production quality and the production efficiency of an adhesive product are effectively improved, the technical innovation and the product innovation of the adhesive and products thereof are driven, the industry development is promoted, and the economic growth is promoted.
Drawings
FIG. 1 is a 40-fold magnified view of an activated heavy calcium carbonate prepared according to the present invention under a microscope.
Detailed Description
The following examples illustrate the invention in more detail, but the scope of the invention is not limited to the examples.
Example 1:
two turbine airflow classifiers are connected in series to carry out two-stage turbine airflow classification on the heavy calcium carbonate, and the particle size range of the fine powder product obtained after classification is obviously narrowed, and the particle size is reduced; through the plurality of powder collecting chambers, the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working state of each powder collecting chamber so as to collect powder; meanwhile, off-line ash removal can be realized.
Adding the powder into a reaction kettle, controlling the temperature of the reaction kettle at 105 ℃, and stirring at a high speed for 3 min; adding stearate into the reaction kettle, controlling the temperature at 125 ℃, and stirring at a high speed for 3 min. Adding aluminate into the reaction kettle, controlling the temperature at 135 ℃, and stirring at low speed for 3min to obtain the active heavy calcium carbonate.
The weight ratio of the heavy calcium carbonate to the stearate to the aluminate is 100: 0.5: 0.5.
example 2:
two turbine airflow classifiers are connected in series to carry out two-stage turbine airflow classification on the heavy calcium carbonate, and the particle size range of the fine powder product obtained after classification is obviously narrowed, and the particle size is reduced; through the plurality of powder collecting chambers, the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working state of each powder collecting chamber so as to collect powder; meanwhile, off-line ash removal can be realized.
Adding the powder into a reaction kettle, controlling the temperature of the reaction kettle at 105 ℃, and stirring at a high speed for 3 min; adding stearate into the reaction kettle, controlling the temperature at 125 ℃, and stirring at a high speed for 3 min. Adding aluminate into the reaction kettle, controlling the temperature at 135 ℃, and stirring at low speed for 3min to obtain the active heavy calcium carbonate.
The weight ratio of the heavy calcium carbonate to the stearate to the aluminate is 100: 0.2: 0.2.
example 3:
two turbine airflow classifiers are connected in series to carry out two-stage turbine airflow classification on the heavy calcium carbonate, and the particle size range of the fine powder product obtained after classification is obviously narrowed, and the particle size is reduced; through the plurality of powder collecting chambers, the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working state of each powder collecting chamber so as to collect powder; meanwhile, off-line ash removal can be realized.
Adding the powder into a reaction kettle, controlling the temperature of the reaction kettle at 105 ℃, and stirring at a high speed for 3 min; adding stearate into the reaction kettle, controlling the temperature at 125 ℃, and stirring at a high speed for 3 min. Adding aluminate into the reaction kettle, controlling the temperature at 135 ℃, and stirring at low speed for 3min to obtain the active heavy calcium carbonate.
The weight ratio of the heavy calcium carbonate to the stearate to the aluminate is 100: 0.8: 0.8.
example 4:
two turbine airflow classifiers are connected in series to carry out two-stage turbine airflow classification on the heavy calcium carbonate, and the particle size range of the fine powder product obtained after classification is obviously narrowed, and the particle size is reduced; through the plurality of powder collecting chambers, the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working state of each powder collecting chamber so as to collect powder; meanwhile, off-line ash removal can be realized.
Adding the powder into a reaction kettle, controlling the temperature of the reaction kettle at 105 ℃, and stirring at a high speed for 3 min; adding stearate into the reaction kettle, controlling the temperature at 125 ℃, and stirring at a high speed for 3 min. Adding aluminate into the reaction kettle, controlling the temperature at 135 ℃, and stirring at low speed for 3min to obtain the active heavy calcium carbonate.
The weight ratio of the heavy calcium carbonate to the stearate to the aluminate is 100: 1: 1.
example 5:
two turbine airflow classifiers are connected in series to carry out two-stage turbine airflow classification on the heavy calcium carbonate, and the particle size range of the fine powder product obtained after classification is obviously narrowed, and the particle size is reduced; through the plurality of powder collecting chambers, the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working state of each powder collecting chamber so as to collect powder; meanwhile, off-line ash removal can be realized.
Adding the powder into a reaction kettle, controlling the temperature of the reaction kettle at 100 ℃, and stirring at a high speed for 2 min; adding aluminate into the reaction kettle, controlling the temperature at 120 ℃, and stirring at high speed for 2 min. Adding stearate into the reaction kettle, controlling the temperature at 140 ℃, and stirring at a low speed for 2min to obtain the active heavy calcium carbonate.
The weight ratio of the heavy calcium carbonate to the stearate to the aluminate is 100: 0.5: 0.5.
example 6:
two turbine airflow classifiers are connected in series to carry out two-stage turbine airflow classification on the heavy calcium carbonate, and the particle size range of the fine powder product obtained after classification is obviously narrowed, and the particle size is reduced; through the plurality of powder collecting chambers, the air inlet valve and the air outlet valve of each powder collecting chamber are controlled by the controller to realize the switching of the working state of each powder collecting chamber so as to collect powder; meanwhile, off-line ash removal can be realized.
Adding the powder into a reaction kettle, controlling the temperature of the reaction kettle at 110 ℃, and stirring at a high speed for 5 min; adding stearate into the reaction kettle, controlling the temperature at 130 ℃, and stirring at a high speed for 5 min. Adding aluminate into the reaction kettle, controlling the temperature at 140 ℃, and stirring at low speed for 5min to obtain the active heavy calcium carbonate.
The weight ratio of the heavy calcium carbonate to the stearate to the aluminate is 100: 0.5: 0.5.
in the above examples, the ground calcium carbonate had a particle size of 6 μm or less, and the content of particles having a particle size of 2 μm or less was 32% or more of the total content.
The effect of modifying ground calcium carbonate was evaluated by the activation ratio, and the activated ground calcium carbonate prepared by modification of the above examples 1 to 6 had the following activation ratio:
| numbering | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Activation ratio% | 89 | 50 | 57 | 49 | 47 | 73 |
From the above table, the weight ratio of the heavy calcium carbonate, the stearate and the aluminate ester is 100: 0.5: at 0.5, the active heavy calcium carbonate has the best modification effect and the highest activation rate.
Fig. 1 is a 40-fold magnified microscope image of the activated ground calcium carbonate prepared in example 1, which has smaller particle size, smooth surface, less tendency to agglomerate, and good dispersibility.
The activated heavy calcium carbonate and the unmodified heavy calcium carbonate prepared in examples 1 to 6 are used as comparative examples, and are filled into the same adhesive according to the same formula and processing technology, and the product performance is respectively tested, and the results are as follows:
therefore, compared with the adhesive added with unmodified ground calcium carbonate, the adhesive added with the active ground calcium carbonate is obviously improved in the aspects of cohesive force and water-resistant stability.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application.
Claims (8)
1. The preparation method of the active heavy calcium carbonate is characterized by comprising the following steps:
step 1: carrying out two-stage turbine airflow classification on the heavy calcium carbonate, wherein the granularity range of the fine powder product obtained after classification is obviously narrowed, and the granularity is reduced;
step 2: collecting powder by adopting a chamber-divided powder collecting technology;
and step 3: adding the powder collected in the step 1 into a reaction kettle, controlling the temperature at 100 ℃ and 110 ℃, and stirring;
and 4, step 4: adding the auxiliary agent 1, controlling the temperature at 120-;
and 5: adding the auxiliary agent 2 into the reaction kettle, controlling the temperature at 135 ℃ and 140 ℃, and stirring to obtain the active heavy calcium carbonate;
wherein the auxiliary agent 1 is stearate, and the auxiliary agent 2 is aluminate; the weight ratio of the heavy calcium carbonate to the auxiliary agent 1 to the auxiliary agent 2 is (100: 0.2-1): 0.2-1.
2. The method for preparing activated heavy calcium carbonate according to claim 1, wherein the two-stage turbine airflow classification is realized by connecting two turbine airflow classifiers in series by using a narrow-stage two-stage turbine airflow classifier.
3. The method for preparing activated heavy calcium carbonate according to claim 1, wherein the chamber-divided dust collection technology is designed to have a plurality of dust collection chambers, and the controller controls the air inlet valve and the air outlet valve of each dust collection chamber to switch the working states of the respective dust collection chambers, so as to achieve off-line dust removal.
4. The method for preparing activated heavy calcium carbonate according to claim 1, wherein the weight part ratio of the heavy calcium carbonate to the auxiliary agent 1 to the auxiliary agent 2 is 100: 0.5: 0.5.
5. the method for preparing activated heavy calcium carbonate according to claim 1, wherein the stirring speed in step 3 and step 4 is higher than the stirring speed in step 5.
6. The method for preparing activated heavy calcium carbonate according to claim 1, wherein the stirring time of the steps 3, 4 and 5 is 2-5 min.
7. The method for preparing activated heavy calcium carbonate according to claim 6, wherein the temperature of the step 3 is controlled at 105 ℃, and the stirring time is 3 min; the temperature of the step 4 is controlled at 125 ℃, and the stirring time is 3 min; and in the step 5, the temperature is controlled at 135 ℃, and the stirring time is 3 min.
8. The process for producing activated ground calcium carbonate according to claim 1, wherein the ground calcium carbonate has a particle size of 6 μm or less, and the content of particles having a particle size of 2 μm or less is 32% or more of the total content.
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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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204933112U (en) * | 2015-09-17 | 2016-01-06 | 江苏群鑫粉体科技股份有限公司 | A kind of locellus receives powder device |
| CN205008241U (en) * | 2015-09-10 | 2016-02-03 | 江苏群鑫粉体科技股份有限公司 | Narrow rank two -stage turbine air current grader grading system |
| WO2017121675A1 (en) * | 2016-01-14 | 2017-07-20 | Omya International Ag | Treatment of surface-reacted calcium carbonate |
| CN108659575A (en) * | 2018-05-28 | 2018-10-16 | 池州市金艺化工有限公司 | A kind of superfine heavy calcium carbonate filler and preparation method thereof |
-
2020
- 2020-06-05 CN CN202010504421.3A patent/CN111574852A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205008241U (en) * | 2015-09-10 | 2016-02-03 | 江苏群鑫粉体科技股份有限公司 | Narrow rank two -stage turbine air current grader grading system |
| CN204933112U (en) * | 2015-09-17 | 2016-01-06 | 江苏群鑫粉体科技股份有限公司 | A kind of locellus receives powder device |
| WO2017121675A1 (en) * | 2016-01-14 | 2017-07-20 | Omya International Ag | Treatment of surface-reacted calcium carbonate |
| CN108659575A (en) * | 2018-05-28 | 2018-10-16 | 池州市金艺化工有限公司 | A kind of superfine heavy calcium carbonate filler and preparation method thereof |
Cited By (2)
| 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 |
| CN116925573B (en) * | 2023-07-20 | 2024-04-05 | 浙江钦堂钙业有限公司 | Activated modified heavy calcium carbonate and preparation method thereof |
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